Pyridine → Phenyl 5-ethyl-1,3,4-thiadiazol-2-ylcarbamate

HRID 1182118

反応式

HRID 1182118 の反応式
[CH2:1]([C:3]1[S:7][C:6]([NH2:8])=[N:5][N:4]=1)[CH3:2].N1C=CC=CC=1.[C:15]1([O:21][C:22](Cl)=[O:23])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>ClCCl>[C:15]1([O:21][C:22](=[O:23])[NH:8][C:6]2[S:7][C:3]([CH2:1][CH3:2])=[N:4][N:5]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 15891Phenyl chloroformateHCID 264442-Amino-5-ethyl-1,3,4-thiadiazole

生成物 1

HCID 66876196Phenyl 5-ethyl-1,3,4-thiadiazol-2-ylcarbamate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 5-Ethyl-[1,3,4]thiadiazol-2-ylamine (2.5 g, 19.4 mmol) and pyridine (1.72 ml, 21.3 mmol) in dichloromethane (70 ml) is cooled to −70° C. and treated with a solution of phenylchloroformate (2.45 ml, 19.6 mmol) in dichloromethane (10 ml) dropwise. The reaction mixture is allowed to warm to ambient temperature and stirred for 3 hours during which a precipitate forms. The precipitate is collected by filtration, and dried under vacuum to afford (5-Ethyl-[1,3,4]thiadiazol-2-yl)-carbamic acid phenyl ester as white solid. [M+H] 250.15

後処理

  1. filtrationThe precipitate is collected by filtration
  2. customdried under vacuum

出典と根拠

ORDレコード
ord-8591886e53384eb2be27eb0b9706c3b2
出典データセット
uspto-grants-2007_10
特許番号
US07288537B2

関連ノート

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