Chlorotrimethylsilane → {4-[4-(5-methoxy-1H-indol-3-yl)piperidine-1-yl]-1-phenylcyclohexyl}-dimethylamine dihydrochloride

HRID 2357437노트

반응식

HRID 2357437 반응식
C1(N)C(F)=C(F)C(F)=C(N)C=1F.[ClH:13].Cl.[CH3:15][O:16][C:17]1[CH:18]=[C:19]2[C:23](=[CH:24][CH:25]=1)[NH:22][CH:21]=[C:20]2[CH:26]1[CH2:31][CH2:30][N:29]([CH:32]2[CH2:37][CH2:36][C:35]([N:44]([CH3:46])[CH3:45])([C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=3)[CH2:34][CH2:33]2)[CH2:28][CH2:27]1.[Cl:47][Si](C)(C)C>CC(CC)=O>[ClH:47].[ClH:13].[CH3:15][O:16][C:17]1[CH:18]=[C:19]2[C:23](=[CH:24][CH:25]=1)[NH:22][CH:21]=[C:20]2[CH:26]1[CH2:27][CH2:28][N:29]([CH:32]2[CH2:33][CH2:34][C:35]([N:44]([CH3:45])[CH3:46])([C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=3)[CH2:36][CH2:37]2)[CH2:30][CH2:31]1

참가 물질

5

반응물 3

HCID 6397ChlorotrimethylsilaneHCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 10029113{4-[4-(5-methoxy-1H-indol-3-yl)piperidine-1-yl]-1-phenylcyclohexyl}-dimethylamine

생성물 1

HCID 10029112{4-[4-(5-methoxy-1H-indol-3-yl)piperidine-1-yl]-1-phenylcyclohexyl}-dimethylamine dihydrochloride

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

To prepare the dihydrochloride the polar diastereoisomer of {4-[4-(5-methoxy-1H-indol-3-yl)piperidine-1-yl]-1-phenylcyclohexyl}-dimethylamine (170 mg, 0.4 mmole) was dissolved in ethyl methyl ketone (5 ml) and chlorotrimethylsilane (125 μl, 1.0 mmole) was added. The solid thereby formed was filtered off and dried. The polar {4-[4-(5-methoxy-1H-indol-3-yl)piperidine-1-yl]-1-phenylcyclohexyl}-dimethylamine dihydrochloride was thereby obtained as a colourless solid with an m.p. of 201°-203° C. in a yield of 200 mg (Example 8).

후처리

  1. customThe solid thereby formed
  2. filtrationwas filtered off
  3. customdried

출처 및 근거

ORD 기록
ord-ba6d2c0f71c84f17bd2bdecc1785a5c4
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07759385B2

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