Triethylamine → 1-(1-Methylpiperidin-4-yl)-4-((1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)methylsulfonyl)piperazine

HRID 1643470

반응식

HRID 1643470 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH2:4][CH2:3]1.C(N(CC)CC)C.[F:21][C:22]([F:44])([F:43])[C:23]1[CH:24]=[C:25]([S:29]([N:32]2[CH2:37][CH2:36][CH2:35][CH2:34][CH:33]2[CH2:38][S:39](Cl)(=[O:41])=[O:40])(=[O:31])=[O:30])[CH:26]=[CH:27][CH:28]=1>C(Cl)Cl>[CH3:1][N:2]1[CH2:3][CH2:4][CH:5]([N:8]2[CH2:13][CH2:12][N:11]([S:39]([CH2:38][CH:33]3[CH2:34][CH2:35][CH2:36][CH2:37][N:32]3[S:29]([C:25]3[CH:26]=[CH:27][CH:28]=[C:23]([C:22]([F:44])([F:21])[F:43])[CH:24]=3)(=[O:31])=[O:30])(=[O:40])=[O:41])[CH2:10][CH2:9]2)[CH2:6][CH2:7]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 5663241-(1-Methyl-4-piperidinyl)piperazineHCID 59367748HCID 59367748, 화합물

생성물 1

HCID 462049761-(1-Methylpiperidin-4-yl)-4-((1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)methylsulfonyl)piperazine수율 30%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

1-(1-Methyl-4-piperidinyl)piperazine (1.126 mmol) was dissolved in methylene chloride (7 ml), the solution was cooled in an ice bath and triethylamine (2.8 mmol) and (1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)methanesulfonic acid chloride (dissolved in methylene chloride (3 ml)) were added. The mixture was stirred for 16 h, during which it was allowed to warm slowly to room temperature. The reaction mixture was diluted with methylene chloride and washed with water and the organic phase was dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography (silica gel) with methylene chloride/methanol (19:1). Yield: 30%. MS, Rt=2.4 min, m/z=553.0 [MH]+

후처리

  1. temperaturethe solution was cooled in an ice bath
  2. washwashed with water
  3. dry with materialthe organic phase was dried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by column chromatography (silica gel) with methylene chloride/methanol (19:1)

출처 및 근거

ORD 기록
ord-64b94bdc6da8478e9d722c226b99b3b0
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119805B2

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