Hydrochloric Acid → HC Yellow No. 2

HRID 1721162

反応式

HRID 1721162 の反応式
C(=O)([O-])[O-].[Ca+2].[N+:6]([C:9]1[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=1[NH2:11])([O-:8])=[O:7].ClC([O:19][CH2:20][CH2:21]Cl)=O.Cl>COCCOC.O>[OH:19][CH2:20][CH2:21][NH:11][C:10]1[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=1[N+:6]([O-:8])=[O:7]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 69462-NitroanilineHCID 10112Calcium CarbonateHCID 123052-Chloroethyl chloroformate

生成物 1

HCID 78637HC Yellow No. 2

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
80 °C

実験手順

60.1 g of calcium carbonate are added to a solution of 138.1 g of 2-nitroaniline in 360 g of monoethylene glycol dimethylether and 60 g of water. 150.0 g of 2-chloroethyl chloroformate are then metered in at 80° C. and the reaction is brought to completion by subsequent stirring at 80° C. 100 g of water and 8.7 g of 35% strength hydrochloric acid are then added, up to a pH of 1, and the lower aqueous phase is separated off. The upper organic phase is diluted with 90 g of monoethylene glycol dimethylether, and 370.6 g of a 50% strength potassium hydroxide solution are added at 15° C. The reaction mixture is then heated to 85° C. and subsequently stirred at 85° C. for 4 hours. Thereafter, 250 g of water are added and the lower salt-containing aqueous phase is separated off. First 500 g of water and then 9 g of 10% strength sulphuric acid are added to the yellow-red organic phase, up to a pH of 8.5. After the monoethylene glycol dimethyl ether has been distilled off and the residue has been cooled to 10° C., the product is obtained in the form of yellow-red crystals.

後処理

  1. customare then metered in at 80° C.
  2. customthe lower aqueous phase is separated off
  3. additionThe upper organic phase is diluted with 90 g of monoethylene glycol dimethylether, and 370.6 g of a 50% strength potassium hydroxide solution
  4. additionare added at 15° C
  5. temperatureThe reaction mixture is then heated to 85° C.
  6. stirringsubsequently stirred at 85° C. for 4 hours
  7. additionThereafter, 250 g of water are added
  8. additionthe lower salt-containing aqueous phase
  9. customis separated off
  10. additionFirst 500 g of water and then 9 g of 10% strength sulphuric acid are added to the yellow-red organic phase, up to a pH of 8.5
  11. distillationAfter the monoethylene glycol dimethyl ether has been distilled off
  12. temperaturethe residue has been cooled to 10° C.
  13. customthe product is obtained in the form of yellow-red crystals

出典と根拠

ORDレコード
ord-5da6d9246c2b4dd7898d7a8b888bf204
出典データセット
uspto-grants-1996_04
特許番号
US05508467

関連ノート

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