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| CAS号 [364-00-1] 生产工艺。 2-乙砜基-5-三氟甲基硝基苯 |
CAS号 [364-00-1] 生产工艺。 2-乙砜基-5-三氟甲基硝基苯
CAS名：Benzene, 1-(ethylsulfonyl)-2-nitro-4-(trifluoromethyl)- 历史参考文献：待检索。
用途：冰染重氮组分19. LookChem网登录2家。 反应类别：氯被乙砜基取代。
BIOS 986, 293-294.（=胶卷PB 77764）。 1-Nitro-2-ethanesulphonyl-5-trifluoromethylbenzene
(Nitro fast Golden Orange GR)
I.G. Hoechst. 英国人译自德文（无资料来源）。
反应式：本人有加注。德文原件暂未找到！（英译文应该是2次文献，日文和中文译文应该是3次文献了！）。
Dr. Shirer supplied the following, dated 1936年3月30日，as the work of a Dr. Schimellschmidt.
Method:
115 kg. Ethanesulphinic acid (43.3% = 105% of
theory), 50 kg. methanol and 113 kg.
Nitro RD base are stirred together and boiled under reflux condenser for 20
hours. At first, temperature is 78℃; towards end of reaction, it is falls to 75℃. Cool
to 70℃. and run in
200 kg. water (70℃.). At 50℃. whilst still stirring, blow out on to a
suction filter, and wash with cold water, until the filtrate is no longer
yellow. The dry product weighs 138.5 kg.
Average purity 99% M.W. 283. i.e. Yield 92%
of theory. M.P. 115-117℃. (crystallized).
FIAT 1313, 223-224.（=胶卷PB 85172）。2-Nitro-4-trifluoromethylphenyl ethylsulfone.
美国人译自德文（无资料来源）。
Nitro Fast Golden Orange GR. Plant capacity: 6 tons.
Equipment: 1) Iron vessel, 3 cu.m., with
jacket, anchor stirring and reflux condenser;
2) vertical centrifuge, capacity: 150 kg.
Materials used per ton: “Nitro RD” 850 kg。
Etanesulfinic acid 560 kg。
Methanol 920 kg。
By-products produced: Methanol of 95% strength 525 kg.
Service requirements per ton of product: Electricity
400 kg。 Steam
8 tons。 Water
600 cu.m。 Air
1000 cu.m.
Procedure:
In (1) 850 kg. of sodium ethanesulfinate,
calculated as 100%, in form of a thick paste,
700 kg. of methanol and 647 kg. of “Nitro RD” are heated for 24-30 hours
at about 75℃. at the
reflux condenser. “Nitro GR”
crystallizes in form of light yellow crystals.
The mixture is cooled to room temperature and the crystal paste is
pressed into (2). The dark methanol
liquor is collected in casks. The
crystals are washed 2-3 times with water until the wash liquor is
colorless. Yield: 760 kg. = 93.5% of
theory.
The methanol containing mother liquor is
distilled in (1). A methanol of about
90-95% strength is obtained. The smeary
residue is pressed from the still into the sewer. Yield: 400 kg. of methanol.
Control:
Test for completeness of reaction by addition of water. Determination of the freezing point of “Nitro
RD”. Determination of the melting point
of :Nitro GR.
Quality:
“Nitro RD”: boiling point 110℃. at 15 mm Hg, Specific gravity 1.54, freezing point -5.8 to -6.3℃.
Ethanesulfinic acid: about 45-50%
strength.
“Nitro GR” = Nitro Fast Golden Orange GR:
melting point 114-115℃. recrystallized 116-117℃.
细田豊 《理论制造染料化学》 1957年。 P. 651. (1) エタンスルフィン酸法。 译自PB 85172.
エタンスルフィン酸ソ- ダ350 kg（抄注： 应为850 kg），メタノ- ル700 kgおよび4-クロル-3-ニトロ-1-ベンゾトリフルオリド647 kgを还流下约750で24-30 h加热し，室温まで冷して结晶を滤洗する。3-ニトロ-4-エタンスルホニルベンゾトリフルオリド760 kg，收率93.5%。
张澍声 《精细化工中间体工业生产技术》 1996年。 P. 16. 2-乙基砜基-5-三氟甲基硝基苯。 译自BIOS 986, 293.
115 kg 乙烷亚磺酸，50 kg甲醇和113 kg 硝基RD Base（即2-氯-5-三氟甲基硝基苯）在一起搅拌，沸腾回流20小时。起初温度为78℃，至反应末期降到75℃。冷却到70℃，加入200 kg 70℃的水。在50℃于搅拌下送往抽滤，冷水洗涤，直至滤液不变黄。干燥后重量138 kg，纯度平均99%，收率92%。重结晶后熔点115-117℃.。
抄注：读者同志，你相信德文原件还是相信译文？如果这类资料有点用，建议还是看原文吧（一手资料）。
陈忠源 2018年11月12日星期一。 文章作者：陈忠源 |
