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Potassium Carbonate → Carbamic acid, (4-amino-2-methyl-5-nitrophenyl)-, 2-chloroethyl ester

HRID 980418
ノート
印刷プレビュー

反応式

HRID 980418 の反応式
[CH3:1][C:2]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:3]=1[NH2:4].C(=O)([O-])[O-].[K+].[K+].O1CCOCC1.[Cl:25][CH2:26][CH2:27][O:28][C:29](Cl)=[O:30]>O>[CH3:1][C:2]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:3]=1[NH:4][C:29](=[O:30])[O:28][CH2:27][CH2:26][Cl:25]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 123052-Chloroethyl chloroformateHCID 312751,4-DioxaneHCID 54879442-Methyl-5-nitrobenzene-1,4-diamine

生成物 1

HCID 14774569Carbamic acid, (4-amino-2-methyl-5-nitrophenyl)-, 2-chloroethyl ester

試薬・触媒・溶媒 1

HCID 962Water
溶媒

反応条件

温度
90 °C

実験手順

0.6 mol (100 g) of 2-methyl-4-amino-5-nitroaniline and 0.36 mol (50 g) of potassium carbonate are introduced into 500 ml of dioxane to which 145 ml of water have been added. The mixture is brought to 90° C., while stirring, and 0.6 mol (86 g) of chloroethylchloroformate is added a little at a time, in the course of 10 minutes. When the addition has ended, heating at 90° C. is continued for 10 minutes and the reaction mixture is cooled to 15° C. and the expected product is filtered off with suction. After being washed with a little dioxane and then with water and alcohol, the product is recrystallised from dioxane and then dried in vacuo. It has a melting point of 192° C.

後処理

  1. additionhave been added
  2. customis brought to 90° C.
  3. customin the course of 10 minutes
  4. additionWhen the addition
  5. temperaturethe reaction mixture is cooled to 15° C.
  6. filtrationthe expected product is filtered off with suction
  7. washAfter being washed with a little dioxane
  8. customwith water and alcohol, the product is recrystallised from dioxane
  9. customdried in vacuo

出典と根拠

ORDレコード
ord-7265f95b274042d98f6baa66fcdd38b2
出典データセット
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04637821

反応ノート

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