Hydrochloric Acid → 3-(3-(((7S)-3,4-dimethoxy-7-bicyclo(4.2.0)octa-1,3,5-trienyl)methylamino)propyl)-7,8-dimethoxy-2,5-dihydro-1H-3-benzazepin-4-one;hydrochloride

HRID 423131노트

반응식

HRID 423131 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C@@H:7]([CH2:13][NH:14][CH2:15][CH2:16][CH2:17][N:18]1[C:24](=[O:25])[CH2:23][C:22]3[CH:26]=[C:27]([O:32][CH3:33])[C:28]([O:30][CH3:31])=[CH:29][C:21]=3[CH2:20][CH2:19]1)[CH2:6]2.[ClH:34]>C(#N)C.C(OCC)C>[ClH:34].[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C@@H:7]([CH2:13][NH:14][CH2:15][CH2:16][CH2:17][N:18]1[C:24](=[O:25])[CH2:23][C:22]3[CH:26]=[C:27]([O:32][CH3:33])[C:28]([O:30][CH3:31])=[CH:29][C:21]=3[CH2:20][CH2:19]1)[CH2:6]2

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 10389261N-Demethylivabradine

생성물 1

HCID 666726993-(3-(((7S)-3,4-dimethoxy-7-bicyclo(4.2.0)octa-1,3,5-trienyl)methylamino)propyl)-7,8-dimethoxy-2,5-dihydro-1H-3-benzazepin-4-one;hydrochloride수율 72.1%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6342Acetonitrile용매

실험 절차

300 mg (0.65 mmol) of the amine obtained in Example 2, Step 2, are dissolved in 10 mL of acetonitrile. To the resulting solution there is added 0.65 mL (1.3 mmol, 2 equivalents) of 2M hydrochloric acid solution in diethyl ether. Stirring is carried out at 25° C. for 15 minutes, and then evaporation to dryness. The product is crystallised from 20 mL of acetone. The solid is filtered off and dried. 230 mg of white crystals are obtained.

후처리

  1. customevaporation to dryness
  2. customThe product is crystallised from 20 mL of acetone
  3. filtrationThe solid is filtered off
  4. customdried

출처 및 근거

ORD 기록
ord-2d9610d533be42abacb334f404b541fb
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101747B2

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