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Hydrochloric Acid → HCID 25206130, 화합물

HRID 387640
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HRID 387640 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 25206131HCID 25206131, 화합물

생성물 1

HCID 25206130HCID 25206130, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-fdfb5a0a068a429bbc0af424a5b3f783
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372864B2

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