Hydrochloric Acid → N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]amino}propyl]-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxamide hydrochloride

HRID 387629노트

반응식

HRID 387629 반응식
[CH2:1]([C@H:8]([NH:24][C:25]([C:27]1[C:28]2[CH2:29][CH2:30][N:31]([CH:38]([CH2:42][CH2:43][CH3:44])[CH2:39][CH2:40][CH3:41])[C:32](=[O:37])[C:33]=2[CH:34]=[CH:35][CH:36]=1)=[O:26])[C@H:9]([OH:23])[CH2:10][NH:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:22])([F:21])[F:20])[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:45]>C(OCC)C.O1CCOCC1>[ClH:45].[CH2:1]([C@H:8]([NH:24][C:25]([C:27]1[C:28]2[CH2:29][CH2:30][N:31]([CH:38]([CH2:42][CH2:43][CH3:44])[CH2:39][CH2:40][CH3:41])[C:32](=[O:37])[C:33]=2[CH:34]=[CH:35][CH:36]=1)=[O:26])[C@H:9]([OH:23])[CH2:10][NH:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:21])([F:22])[F:20])[CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 25206291N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]amino}propyl]-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxamide

생성물 1

HCID 25206290N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]amino}propyl]-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxamide hydrochloride

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane용매

실험 절차

38 mg of N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]amino}propyl]-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxamide are dissolved in 8 cm3 of ethyl ether at a temperature close to 20° C. 0.2 cm3 of a 4M hydrochloric acid solution in dioxane is added while stirring under argon. The reaction mixture precipitates. The stirring is stopped in order to remove the supernatant, then 5 cm3 of ethyl ether are again added. This operation is carried out 3 times. The last suspension is then concentrated under reduced pressure (5 kPa). 26 mg of N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]amino}propyl]-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxamide hydrochloride (1:1) are obtained in the form of a white solid.

후처리

  1. customclose to 20° C
  2. customThe reaction mixture precipitates
  3. customto remove the supernatant
  4. addition5 cm3 of ethyl ether are again added
  5. concentrationThe last suspension is then concentrated under reduced pressure (5 kPa)

출처 및 근거

ORD 기록
ord-231a99c7c7ae4209a877651942c6f7c6
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372864B2

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