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

HRID 2357436ノート

反応式

HRID 2357436 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

To prepare the dihydrochloride the non-polar diastereoisomer of {4-[4-(5-methoxy-1H-indol-3-yl)piperidine-1-yl]-1-phenylcyclohexyl}-dimethylamine (590 mg, 1.37 mmole) was dissolved in ethyl methyl ketone (7 ml) and chlorotrimethylsilane (435 μl, 3.4 mmole) was added. The solid thereby formed was filtered off and dried. The non-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 224°-226° C. in a yield of 690 mg (100%)(Example 7).

後処理

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

出典と根拠

ORDレコード
ord-e7f37b9caef04d1d97f30217b336dd21
出典データセット
uspto-grants-2010_07
特許番号
US07759385B2

反応ノート

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