Triethylamine → HCID 19045808、化合物

HRID 1781518ノート

反応式

HRID 1781518 の反応式
[NH2:1][CH2:2][C:3]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:4][CH2:5][CH2:6][N:7]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:9][CH2:8]1.C(N(CC)CC)C.[CH3:38][S:39]([Cl:42])(=[O:41])=[O:40]>C(Cl)Cl>[ClH:42].[C:25]1([C:3]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)([CH2:2][NH:1][S:39]([CH3:38])(=[O:41])=[O:40])[CH2:4][CH2:5][CH2:6][N:7]2[CH2:12][CH2:11][CH:10]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH2:9][CH2:8]2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 9865634HCID 9865634、化合物

生成物 1

HCID 19045808HCID 19045808、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-amino-4,4-diphenyl-1-(4-phenylpiperidino)pentane (0.4 g) and triethylamine (0.42 ml) in methylene chloride (15 ml) was added methanesulfonyl chloride (0.1 ml) dropwise under ice-cooling and stirring. After completion of dropwise addition, the mixture was returned to room temperature and stirred for another 3 hours. This reaction mixture was washed with water, dried over anhydrous sodium sulfate, and concentrated to dryness. The group was purified by silica gel column chromatography to provide the hydrochloride of the title compound (0.25 g) as colorless powder.

後処理

  1. temperaturecooling
  2. additionAfter completion of dropwise addition
  3. customwas returned to room temperature
  4. stirringstirred for another 3 hours
  5. washThis reaction mixture was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated to dryness
  8. customThe group was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f481802e6a614778937029828a5a0491
出典データセット
uspto-grants-1997_05
特許番号
US05633248

反応ノート

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