Hydrochloric Acid → HCID 86646923, 화합물

HRID 221497

반응식

HRID 221497 반응식
[CH2:1]([O:3][C:4]([O:6][CH2:7][CH2:8][O:9][C:10]([C:12]1[N:13]=[C:14]([C:43]([F:46])([F:45])[F:44])[N:15]2[CH2:20][CH2:19][N:18]([C:21](=[O:42])[CH2:22][C@H:23]([NH:34]C(OC(C)(C)C)=O)[CH2:24][C:25]3[CH:30]=[C:29]([F:31])[C:28]([F:32])=[CH:27][C:26]=3[F:33])[CH2:17][C:16]=12)=[O:11])=[O:5])[CH3:2].[ClH:47]>C(OCC)(=O)C>[ClH:47].[CH2:1]([O:3][C:4]([O:6][CH2:7][CH2:8][O:9][C:10]([C:12]1[N:13]=[C:14]([C:43]([F:44])([F:45])[F:46])[N:15]2[CH2:20][CH2:19][N:18]([C:21](=[O:42])[CH2:22][C@H:23]([NH2:34])[CH2:24][C:25]3[CH:30]=[C:29]([F:31])[C:28]([F:32])=[CH:27][C:26]=3[F:33])[CH2:17][C:16]=12)=[O:11])=[O:5])[CH3:2]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86646922(R)-7-[3-tert-butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyryl]-3-trifluoromethyl-5,6,7,8-tetrahydro-imidazo[1,5-a]pyrazine-1-carboxylic acid (1-ethoxycarbonyloxy)-ethyl ester

생성물 1

HCID 86646923HCID 86646923, 화합물수율 85%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

(R)-7-[3-tert-Butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyryl]-3-trifluoromethyl-5,6,7,8-tetrahydro-imidazo[1,5-a]pyrazine-1-carboxylic acid (1-ethoxycarbonyloxy)-ethyl ester 34a (0.26 g, 0.39 mmol) and 5 mL of ethyl acetate were added into the reaction flask. A solution of 6.5 N hydrochloric acid in 3 mL of ethyl acetate was then added to the flask. The reaction mixture was stirred at room temperature for 6 hours and monitored by thin layer chromatography until the disappearance of the starting materials. The reaction mixture was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound (R)-7-[3-amino-4-(2,4,5-trifluoro-phenyl)-butyryl]-3-trifluoromethyl-5,6,7,8-tetrahydro-imidazo[1,5-a]pyrazine-1-carboxylic acid (1-ethoxycarbonyloxy)-ethyl ester hydrochloride 34 (0.2 g, yield 85%) as a white solid.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customThe resulting residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-52815ee926814c2a8b62cbd6469365da
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207161B2

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