Pyridine → HCID 46180827、化合物

HRID 2380962ノート

反応式

HRID 2380962 の反応式
[Cl:1][C:2]1[CH:29]=[CH:28][C:5]([CH2:6][NH:7][C:8]2[CH:13]=[CH:12][C:11]([C:14]([N:16]3[CH2:21][CH2:20][N:19]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[CH2:18][CH2:17]3)=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[C:30]1([S:36](Cl)(=[O:38])=[O:37])[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.N1C=CC=CC=1.C(O)C(N)(CO)CO>ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][N:7]([C:8]2[CH:9]=[CH:10][C:11]([C:14]([N:16]3[CH2:21][CH2:20][N:19]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[CH2:18][CH2:17]3)=[O:15])=[CH:12][CH:13]=2)[S:36]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)(=[O:38])=[O:37])=[CH:28][CH:29]=1

参加物

6

反応物 4

HCID 1049PyridineHCID 6503Tris(hydroxymethyl)aminomethaneHCID 7369Benzenesulfonyl chlorideHCID 67130576HCID 67130576、化合物

生成物 1

HCID 46180827HCID 46180827、化合物収率 125.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of [4-(4-chloro-benzylamino)-phenyl]-(4-phenyl-piperazin-1-yl)-methanone (30 mg, 0.07 mmol) and phenylsulfonyl chloride (14.2 μl, 0.11 mmol) in anhydrous dichloromethane (1 ml) was added pyridine (7.2 μl, 0.09 mmol) and the reaction was stirred at ambient for 18 hours. PS-trisamine (32 mg, 0.13 mmol) was added and the mixture was agitated for 3 hours then filtered. The filtrate was concentrated in vacuo to afford the title compound as a yellow solid (48 mg, 98% yield). HPLC retention time 7.7 min. Mass spectrum (ES+) m/z 547 (M+H).

後処理

  1. stirringthe mixture was agitated for 3 hours
  2. filtrationthen filtered
  3. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-5c278c5d6f1048868f6350bce6f06752
出典データセット
uspto-grants-2012_09
特許番号
US08258138B2

反応ノート

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