Trifluoroacetic acid → HCID 89719307, 화합물

HRID 63727

반응식

HRID 63727 반응식
[CH3:1][O:2][C:3](=[O:46])[C@@H:4]([NH:23][C:24](=[O:45])[C:25]1[C:30]([Cl:31])=[CH:29][C:28]([O:32][CH2:33][CH2:34][CH2:35][NH:36]C(OC(C)(C)C)=O)=[CH:27][C:26]=1[Cl:44])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13](=[O:22])[C:14]2[C:19]([Cl:20])=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:21])=[CH:8][CH:7]=1.C(O)(C(F)(F)F)=O>ClCCl>[CH3:1][O:2][C:3](=[O:46])[C@@H:4]([NH:23][C:24](=[O:45])[C:25]1[C:26]([Cl:44])=[CH:27][C:28]([O:32][CH2:33][CH2:34][CH2:35][NH2:36])=[CH:29][C:30]=1[Cl:31])[CH2:5][C:6]1[CH:7]=[CH:8][C:9]([NH:12][C:13](=[O:22])[C:14]2[C:19]([Cl:20])=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:21])=[CH:10][CH:11]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 89717547(S)-2-[4-(3-tert-butoxycarbonylaminopropoxy)-2,6-dichlorobenzoylamino]-3-[4-(2,6-dichlorobenzoylamino)phenyl]propionic acid methyl ester

생성물 1

HCID 89719307HCID 89719307, 화합물수율 118.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of (S)-2-[4-(3-tert-butoxycarbonylaminopropoxy)-2,6-dichlorobenzoylamino]-3-[4-(2,6-dichlorobenzoylamino)phenyl]propionic acid methyl ester (7.5 g, 7.98 mmol) in dichloromethane (100 mL) was added an excess of TFA (9.12 g, 5.9 mL, 80 mmol) at room temperature. The resulting solution was stirred for 15 h. Then, the solvent was removed under vacuum and the residue was azeotrophed one time with toluene. After drying under high vacuum, 5.8 g (99%) of (S)-2-[4-(3-aminopropoxy)-2,6-dichlorobenzoylamino]-3-[4-(2,6-dichlorobenzoylamino)phenyl]propionic acid methyl ester was obtained as a white solid. ES(+)-HRMS m/e calcd. for C27H25Cl4N3O5 (M+H)+ 612.0621, obsd. 612.0619.

후처리

  1. customThen, the solvent was removed under vacuum
  2. customAfter drying under high vacuum

출처 및 근거

ORD 기록
ord-c51cf0cc9a4948cf95c67713976f5da1
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447035B2

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