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

HRID 1710668노트

반응식

HRID 1710668 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-6d1b61845b72467198110849ac1dfade
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07790726B2

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