Triethylamine → HCID 19045808, 화합물

HRID 1781518노트

반응식

HRID 1781518 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 9865634HCID 9865634, 화합물

생성물 1

HCID 19045808HCID 19045808, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f481802e6a614778937029828a5a0491
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05633248

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