Trifluoroacetic acid → 1-(Piperidin-4-ylcarbonyl)-4-(6-chloronaphthalen-2-yl-sulfonyl)piperazine Trifluoroacetate

HRID 431527노트

반응식

HRID 431527 반응식
C([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([N:16]2[CH2:21][CH2:20][N:19]([S:22]([C:25]3[CH:34]=[CH:33][C:32]4[C:27](=[CH:28][CH:29]=[C:30]([Cl:35])[CH:31]=4)[CH:26]=3)(=[O:24])=[O:23])[CH2:18][CH2:17]2)=[O:15])[CH2:10][CH2:9]1)(OC(C)(C)C)=O.C1(OC)C=CC=CC=1.[C:44]([OH:50])([C:46]([F:49])([F:48])[F:47])=[O:45]>ClCCl>[F:47][C:46]([F:49])([F:48])[C:44]([OH:50])=[O:45].[NH:8]1[CH2:13][CH2:12][CH:11]([C:14]([N:16]2[CH2:17][CH2:18][N:19]([S:22]([C:25]3[CH:34]=[CH:33][C:32]4[C:27](=[CH:28][CH:29]=[C:30]([Cl:35])[CH:31]=4)[CH:26]=3)(=[O:24])=[O:23])[CH2:20][CH2:21]2)=[O:15])[CH2:10][CH2:9]1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 121120201-(t-Butoxycarbonyl)4-(1-(6-chloronaphth-2-ylsulphonyl)piperazin-4-ylcarbonyl)piperidine

생성물 1

HCID 187613891-(Piperidin-4-ylcarbonyl)-4-(6-chloronaphthalen-2-yl-sulfonyl)piperazine Trifluoroacetate수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirring solution of 1-(1-Boc-piperidin-4-yl-carbonyl)-4-(6-chloronaphthalen-2-ylsulfonyl)piperazine (2.2 g, 4.2 mmol) in dichloromethane (25 mL) was added anisole (2 mL) followed by TFA (25 mL). After 90 min, the solvents were removed in vacuo and the residue was dissolved in a few mL of dichloromethane and diluted with diethyl ether (200 mL). After stirring for 2 h, the suspension was sonicated and filtered and then the solid was washed with diethyl ether and dried in vacuo to give 2.25 g (99%) of a white solid.

후처리

  1. customthe solvents were removed in vacuo
  2. dissolutionthe residue was dissolved in a few mL of dichloromethane
  3. additiondiluted with diethyl ether (200 mL)
  4. customthe suspension was sonicated
  5. filtrationfiltered
  6. washthe solid was washed with diethyl ether
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-51990b05add0475a87b588a561d53a00
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660739B1

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