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Ethoxyacetyl chloride → Tert-butyl 2-({2-chloro-3-[(ethoxyacetyl)amino]quinolin-4-yl}amino)ethylcarbamate

HRID 606065
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HRID 606065 반응식
[CH2:1]([O:3][CH2:4][C:5](Cl)=[O:6])[CH3:2].[NH2:8][C:9]1[C:10]([Cl:30])=[N:11][C:12]2[C:17]([C:18]=1[NH:19][CH2:20][CH2:21][NH:22][C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[CH:16][CH:15]=[CH:14][CH:13]=2>C(#N)C>[Cl:30][C:10]1[C:9]([NH:8][C:5](=[O:6])[CH2:4][O:3][CH2:1][CH3:2])=[C:18]([NH:19][CH2:20][CH2:21][NH:22][C:23](=[O:29])[O:24][C:25]([CH3:27])([CH3:26])[CH3:28])[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 84189Ethoxyacetyl chlorideHCID 86616882Tert-butyl 2-[(3-amino-2-chloroquinolin-4-yl)amino]ethylcarbamate

생성물 1

HCID 86616883Tert-butyl 2-({2-chloro-3-[(ethoxyacetyl)amino]quinolin-4-yl}amino)ethylcarbamate수율 93.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A solution of ethoxyacetyl chloride (857 mg, 6.99 mmol) in acetonitrile (5 mL) was added to solution of tert-butyl 2-[(3-amino-2-chloroquinolin-4-yl)amino]ethylcarbamate (2.14 g, 6.35 mmol) in acetonitrile (20 mL). After five minutes, the solution was cooled in an ice bath and a white precipitate began to form. After one hour, the precipitate was isolated by filtration and dried under vacuum to afford the hydrochloride salt of tert-butyl 2-({2-chloro-3-[(ethoxyacetyl)amino]quinolin-4-yl}amino)ethylcarbamate (2.50 g).

후처리

  1. temperaturethe solution was cooled in an ice bath
  2. customto form
  3. waitAfter one hour
  4. customthe precipitate was isolated by filtration
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-87c4883a99a14edc9dbb2b0855d5d17d
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07915281B2

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