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

HRID 1980749
ノート
印刷プレビュー

反応式

HRID 1980749 の反応式
[CH3:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([N+:9]([O-:11])=[O:10])=[C:4]([NH2:12])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].O1CCOCC1.Cl[C:26]([O:28][CH2:29][CH2:30][Cl:31])=[O:27]>O>[CH3:1][C:2]1[CH:3]=[C:4]([NH2:12])[C:5]([N+:9]([O-:11])=[O:10])=[CH:6][C:7]=1[NH:8][C:26](=[O:27])[O:28][CH2:29][CH2:30][Cl:31]
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 4-methyl-2,5-diamino-nitrobenzene 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 heated to 90° C., whilst stirring, and 0.6 mol (86 g) of chloroethyl chloroformate is then added gradually, in the course of 10 minutes. When the addition has ended, the heating is maintained for 10 minutes at 90° C. The reaction medium is cooled to 15° C. and the desired product is then filtered off. After washing with a small amount of dioxane and then with water and alcohol, the product is recrystallised from dioxane and then dried in vacuo. It melts at 192° C.

後処理

  1. additionhave been added
  2. additionWhen the addition
  3. temperaturethe heating is maintained for 10 minutes at 90° C
  4. temperatureThe reaction medium is cooled to 15° C.
  5. filtrationthe desired product is then filtered off
  6. washAfter washing with a small amount of dioxane
  7. customwith water and alcohol, the product is recrystallised from dioxane
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-7469fa6f88254cf9ba59b18eb10ef7d3
出典データセット
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04511360

反応ノート

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