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Triethylamine → [Tert-butoxycarbonyl-(3-chloro-propyl)-amino]-(4-fluoro-phenyl)-acetic acid methyl ester

HRID 1644816
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HRID 1644816 반응식
[CH3:1][O:2][C:3](=[O:17])[CH:4]([NH:12][CH2:13][CH2:14][CH2:15][Cl:16])[C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=1.[O:18](C(OC(C)(C)C)=O)[C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=O.C(N(CC)CC)C>CN(C=O)C.CCOC(C)=O.O>[CH3:1][O:2][C:3](=[O:17])[CH:4]([N:12]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:18])[CH2:13][CH2:14][CH2:15][Cl:16])[C:5]1[CH:6]=[CH:7][C:8]([F:11])=[CH:9][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 90495Di-tert-butyl dicarbonate2회HCID 66774470(3-Chloro-propylamino)-(4-fluoro-phenyl)-acetic acid methyl ester

생성물 1

HCID 66775166[Tert-butoxycarbonyl-(3-chloro-propyl)-amino]-(4-fluoro-phenyl)-acetic acid methyl ester수율 57.8%

시약·촉매·용매 3

HCID 962Water용매
HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of (3-chloro-propylamino)-(4-fluoro-phenyl)-acetic acid methyl ester (14.34 g) in DMF (40 mL) was added BOC2O (11.44 g) followed by triethylamine (15.9 g) and the resultant mixture was stirred overnight at 60° C. A further 0.25 equivalents of BOC2O was added and the reaction mixture was stirred a further 18 hours. The reaction mixture was diluted with EtOAc (200 mL) and water (150 mL), the phases were separated and the organic phase was washed with 0.5 N HCl solution, water, brine and dried over sodium sulfate. Filtration of the drying agent and evaporation of the volatiles in vacuo afforded crude [tert-butoxycarbonyl-(3-chloro-propyl)-amino]-(4-fluoro-phenyl)-acetic acid methyl ester (10.91 g, MS (ES+): 360.1 (MH+)) as a brown oil which was used in the subsequent reaction without further purification.

후처리

  1. customthe phases were separated
  2. washthe organic phase was washed with 0.5 N HCl solution, water, brine
  3. dry with materialdried over sodium sulfate
  4. filtrationFiltration of the drying agent and evaporation of the volatiles in vacuo

출처 및 근거

ORD 기록
ord-db271ee7537141e6a6c98b51a0027d4e
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08124636B2

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