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

HRID 431527ノート

反応式

HRID 431527 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-51990b05add0475a87b588a561d53a00
出典データセット
uspto-grants-2003_12
特許番号
US06660739B1

反応ノート

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