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

HRID 1661085
ノート
印刷プレビュー

反応式

HRID 1661085 の反応式
[CH2:1]([C@H:8]([NH:24][C:25]([C:27]1[C:28]2[CH:29]=[CH: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[CH:29]=[CH: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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 25204518N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]-amino}propyl]-1-oxo-2-(1-propylbutyl)-1,2-dihydroisoquinoline-5-carboxamide

生成物 1

HCID 67429965N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]amino}propyl]-1-oxo-2-(1-propylbutyl)-1,2-dihydroisoquinoline-5-carboxamide hydrochloride

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒
HCID 31275
1,4-Dioxane
溶媒

実験手順

84 mg of N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]-amino}propyl]-1-oxo-2-(1-propylbutyl)-1,2-dihydroisoquinoline-5-carboxamide are dissolved in 4 cm3 of ethyl ether at a temperature close to 20° C. 0.2 cm3 of a 4M solution of hydrochloric acid in dioxane is added while stirring and under argon. The reaction mixture precipitates. The stirring is stopped. The supernatant is removed and 5 cm3 of ethyl ether are added. This operation is carried out three times. The last suspension is concentrated under reduced pressure (5 kPa). 87 mg of N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]amino}propyl]-1-oxo-2-(1-propylbutyl)-1,2-dihydroisoquinoline-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. customThe supernatant is removed
  4. addition5 cm3 of ethyl ether are added
  5. concentrationThe last suspension is concentrated under reduced pressure (5 kPa)

出典と根拠

ORDレコード
ord-e57830f8a2ee4b49b8ce8b3dfe0ab92a
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08030320B2

反応ノート

読み込み中…

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