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Water → Ethyl 4-chloro-3-cyanophenylcarbamate

HRID 2355759
ノート
印刷プレビュー

反応式

HRID 2355759 の反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[NH2:7][C:8]1[CH:9]=[CH:10][C:11]([Cl:16])=[C:12]([CH:15]=1)[C:13]#[N:14].N1C=CC=CC=1.O>C(Cl)Cl>[Cl:16][C:11]1[CH:10]=[CH:9][C:8]([NH:7][C:2](=[O:3])[O:4][CH2:5][CH3:6])=[CH:15][C:12]=1[C:13]#[N:14]
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 962WaterHCID 1049PyridineHCID 10928Ethyl chloroformateHCID 109972345-Amino-2-chlorobenzonitrile

生成物 1

HCID 60705219Ethyl 4-chloro-3-cyanophenylcarbamate収率 94.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of ethyl chloroformate (3.68 g) in methylene chloride (5 ml) is added dropwise in about 20 minutes to a mixture of 5-amino-2-chlorobenzonitrile (5.2 g) and pyridine (2.77 g) in methylene chloride (75 ml), cooled to 0° C. and maintained in an inert atmosphere. At the end of the addition, the solution is stirred for 1 hour at 0° C. and is then brought to room temperature. At the end of the reaction, the mixture is poured into water (100 ml) and extracted with methylene chloride (2×80 ml); the organic phase is washed with water (2×80 ml), dried with sodium sulphate and concentrated under vacuum. 7.2 g of product are obtained.

後処理

  1. temperaturemaintained in an inert atmosphere
  2. additionAt the end of the addition
  3. customis then brought to room temperature
  4. customAt the end of the reaction
  5. extractionextracted with methylene chloride (2×80 ml)
  6. washthe organic phase is washed with water (2×80 ml)
  7. dry with materialdried with sodium sulphate
  8. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-d304c6e19ad741f489805e226c057952
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07754880B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート