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Methyl chloroformate → (2-Cyclopropylcarbamoyl-phenyl)-carbamic acid methyl ester

HRID 896344
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HRID 896344 반응식
[NH2:1][C:2]1[CH:13]=[CH:12][CH:11]=[CH:10][C:3]=1[C:4]([NH:6][CH:7]1[CH2:9][CH2:8]1)=[O:5].[CH3:14][O:15][C:16](Cl)=[O:17]>O>[CH3:14][O:15][C:16](=[O:17])[NH:1][C:2]1[CH:13]=[CH:12][CH:11]=[CH:10][C:3]=1[C:4](=[O:5])[NH:6][CH:7]1[CH2:8][CH2:9]1
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참가 물질

4

반응물 2

HCID 6586Methyl chloroformateHCID 20600072-amino-N-cyclopropylbenzamide

생성물 1

HCID 20814106(2-Cyclopropylcarbamoyl-phenyl)-carbamic acid methyl ester수율 99.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a slurry of 2-amino-N-cyclopropyl-benzamide (6.7 g, 38.1 mmol) in water was added KHCO3 (9.5 g, 95.1 mmol) followed by careful addition of methylchloroformate (5.88 ml, 76.2 mmol). The mixture was stirred for 12 h then the aqueous layer was extracted with EtOAc. The EtOAc extract was washed with 1N HCl then dried over MgSO4 and concentrated to give 8.9 g (99%) of (2-cyclopropylcarbamoyl-phenyl)-carbamic acid methyl ester.

후처리

  1. extractionthe aqueous layer was extracted with EtOAc
  2. extractionThe EtOAc extract
  3. washwas washed with 1N HCl
  4. dry with materialthen dried over MgSO4
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3a9f0fe3b0a84313a213da891b71d62b
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06919331B2

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