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 387629ノート

反応式

HRID 387629 の反応式
[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

参加物

5

反応物 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

生成物 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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-231a99c7c7ae4209a877651942c6f7c6
出典データセット
uspto-grants-2013_02
特許番号
US08372864B2

反応ノート

読み込み中…