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Hydrochloric Acid → HCID 25206130、化合物

HRID 387640
ノート
印刷プレビュー

反応式

HRID 387640 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:43]=[C:44]([F:46])[CH:45]=1)[CH2:5][C@H:6]([NH:24][C:25]([C:27]1[C:28]2[CH2:29][CH2:30][N:31]([CH2:38][CH2:39][CH2:40][CH2:41][CH3:42])[C:32](=[O:37])[C:33]=2[CH:34]=[CH:35][CH:36]=1)=[O:26])[C@H:7]([OH:23])[CH2:8][NH:9][C:10]1([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:22])([F:21])[F:20])[CH:14]=2)[CH2:12][CH2:11]1.[ClH:47]>C(OCC)C>[ClH:47].[F:1][C:2]1[CH:3]=[C:4]([CH:43]=[C:44]([F:46])[CH:45]=1)[CH2:5][C@H:6]([NH:24][C:25]([C:27]1[C:28]2[CH2:29][CH2:30][N:31]([CH2:38][CH2:39][CH2:40][CH2:41][CH3:42])[C:32](=[O:37])[C:33]=2[CH:34]=[CH:35][CH:36]=1)=[O:26])[C@H:7]([OH:23])[CH2:8][NH:9][C:10]1([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:21])([F:20])[F:22])[CH:14]=2)[CH2:11][CH2:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 25206131HCID 25206131、化合物

生成物 1

HCID 25206130HCID 25206130、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

360 mg of N-[(1S,2R)-1-(3,5-difluorobenzyl)-2-hydroxy-3-({1-[3-(trifluoromethyl)phenyl]cyclopropyl}amino)propyl]-1-oxo-2-pentyl-1,2,3,4-tetrahydroisoquinoline-5-carboxamide are stirred under an inert atmosphere in 6 cm3 of ethyl ether at a temperature close to 5° C. 1.9 cm3 of a 2M solution of hydrochloric acid in ether are added. The solution is concentrated under reduced pressure (5 kPa). Ethyl ether is added. The suspension is stirred then, after stopping the stirring, the supernatant is removed. Ethyl ether is again added. This operation is carried out several times. The last suspension is then concentrated under reduced pressure (5 kPa). 363 mg of N-[(1S,2R)-1-(3,5-difluorobenzyl)-2-hydroxy-3-({1-[3-(trifluoromethyl)phenyl]cyclopropyl}amino)propyl]-1-oxo-2-pentyl-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 5° C
  2. concentrationThe solution is concentrated under reduced pressure (5 kPa)
  3. additionEthyl ether is added
  4. customthe supernatant is removed
  5. additionEthyl ether is again added
  6. concentrationThe last suspension is then concentrated under reduced pressure (5 kPa)

出典と根拠

ORDレコード
ord-fdfb5a0a068a429bbc0af424a5b3f783
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08372864B2

反応ノート

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