1-(1-Methyl-4-piperidinyl)piperazine → 2-[1-(4-Methoxy-2,6-dimethyl-phenylsulfonyl)-piperidin-2-ylmethoxy]-1-[4-(1-methyl-piperidin-4-yl)-piperazin-1-yl]-ethanone

HRID 2090805

반응식

HRID 2090805 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([S:10]([N:13]2[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]2[CH2:19][O:20][CH2:21][C:22](O)=[O:23])(=[O:12])=[O:11])=[C:5]([CH3:25])[CH:4]=1.[CH3:26][N:27]1[CH2:32][CH2:31][CH:30]([N:33]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]2)[CH2:29][CH2:28]1>ClCCl>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([S:10]([N:13]2[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]2[CH2:19][O:20][CH2:21][C:22]([N:36]2[CH2:35][CH2:34][N:33]([CH:30]3[CH2:31][CH2:32][N:27]([CH3:26])[CH2:28][CH2:29]3)[CH2:38][CH2:37]2)=[O:23])(=[O:12])=[O:11])=[C:5]([CH3:25])[CH:4]=1

참가 물질

4

반응물 2

HCID 5663241-(1-Methyl-4-piperidinyl)piperazineHCID 574368002-((1-(4-Methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)methoxy)acetic acid

생성물 1

HCID 249455742-[1-(4-Methoxy-2,6-dimethyl-phenylsulfonyl)-piperidin-2-ylmethoxy]-1-[4-(1-methyl-piperidin-4-yl)-piperazin-1-yl]-ethanone

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

N,N′-Carbonyldiimidazole (114 mg, 0.706 mmol) was added to a solution of 2-((1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)methoxy)acetic acid (250 mg, 0.673 mmol) in dichloromethane (15 ml), and the mixture was stirred for 1 h at room temperature. A solution of 1-(1-methylpiperidin-4-yl)piperazine (123 mg, 0.673 mmol) in dichloromethane (5 ml) was then added, and the reaction mixture was stirred for 15 h at room temperature. The reaction mixture was then extracted with water (20 ml) and saturated sodium chloride solution (20 ml), and the organic phase was dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by flash chromatography using dichloromethane/methanol (97:3→90:10).

후처리

  1. stirringthe reaction mixture was stirred for 15 h at room temperature
  2. extractionThe reaction mixture was then extracted with water (20 ml) and saturated sodium chloride solution (20 ml)
  3. dry with materialthe organic phase was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by flash chromatography

출처 및 근거

ORD 기록
ord-6601b9ab513848f6b96a0bce5eed963b
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08435978B2

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