Pyridine → (4-Chloro-2-hydroxymethyl-phenyl)-carbamic acid ethyl ester

HRID 1710668ノート

反応式

HRID 1710668 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH2:9][OH:10].Cl[C:12]([O:14][CH2:15][CH3:16])=[O:13].N1C=CC=CC=1>C(Cl)Cl.CCOC(C)=O>[CH2:15]([O:14][C:12](=[O:13])[NH:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH2:9][OH:10])[CH3:16]

参加物

6

反応物 3

HCID 1049PyridineHCID 10928Ethyl chloroformateHCID 5867542-Amino-5-chlorobenzyl alcohol

生成物 1

HCID 58834345(4-Chloro-2-hydroxymethyl-phenyl)-carbamic acid ethyl ester

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of (2-amino-5-chloro-phenyl)-methanol (1.58 g, 10 mmol, 1 equiv) in 15 mL of DCM was slowly added ethyl chloroformate (1.05 mL, 1.1 equiv) and pyridine (1.2 mL, 1.5 equiv). After stirring for 1 h, the resultant mixture was diluted with EtOAc and washed with water. The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo to provide the crude product, (4-Chloro-2-hydroxymethyl-phenyl)-carbamic acid ethyl ester (71), which was used in subsequent reactions without further purification.

後処理

  1. washwashed with water
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-6d1b61845b72467198110849ac1dfade
出典データセット
uspto-grants-2010_09
特許番号
US07790726B2

反応ノート

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