Ethyl chloroformate → HCID 14648418、化合物

HRID 1638287ノート

反応式

HRID 1638287 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8](=[O:10])[N:7]([CH2:11][C:12]([N:14]3[CH2:19][CH2:18][CH:17]([OH:20])[CH2:16][CH2:15]3)=[O:13])[C:6]=2[CH:21]=1.[C:22](Cl)(=[O:26])[O:23][CH2:24][CH3:25]>N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8](=[O:10])[N:7]([CH2:11][C:12]([N:14]3[CH2:15][CH2:16][CH:17]([O:20][C:22]([O:23][CH2:24][CH3:25])=[O:26])[CH2:18][CH2:19]3)=[O:13])[C:6]=2[CH:21]=1

参加物

4

反応物 2

HCID 10928Ethyl chloroformateHCID 3082453Hpr 611

生成物 1

HCID 14648418HCID 14648418、化合物収率 81.9%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
80 °C

実験手順

5-Chloro-3-(4-hydroxypiperidinocarbonylmethyl)benzothiazolin-2-one (3.2 g) was dissolved in dry pyridine (15 ml) and the solution was cooled. After ethyl chlorocarbonate (1.5 g) was dropwise added to the solution, the resultant was stirred for 8 hours at 80° C. Pyridine was evaporated off under vacuum from the reaction mixture and the residue was recrystallized from a mixture of chloroform and ethanol to yield the title compound as colorless crystals (3.2 g). mp 196°-197° C.

後処理

  1. temperaturethe solution was cooled
  2. customPyridine was evaporated off under vacuum from the reaction mixture
  3. customthe residue was recrystallized from a mixture of chloroform and ethanol

出典と根拠

ORDレコード
ord-ae96f7b61a1f4a558cf91b40802ca34e
出典データセット
uspto-grants-1989_11
特許番号
US04879301

反応ノート

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