Lawesson's reagent → Ammonia

HRID 551597

反応式

HRID 551597 の反応式
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:13]=[N:14][C:15]([CH2:18][N:19]3[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)=[CH:16][CH:17]=2)=O)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:34])=CC=1>C1COCC1>[NH3:4].[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:13]=[N:14][C:15]([CH2:18][N:19]3[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)=[CH:16][CH:17]=2)=[S:34])[CH2:6][CH2:5]1)([CH3:3])[CH3:2]

参加物

5

反応物 2

HCID 87949Lawesson's reagentHCID 11522780(4-Isopropyl-piperazin-1-yl)-(6-piperidin-1-ylmethyl-pyridin-3-yl)-methanone

生成物 2

HCID 222Ammonia収率 1%HCID 11609917(4-Isopropyl-piperazin-1-yl)-(6-piperidin-1-ylmethylpyridin-3-yl)-methanethione

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of (4-isopropyl-piperazin-1-yl)-(6-piperidin-1-ylmethyl-pyridin-3-yl)-methanone (Example 1, 80 mg, 0.24 mmol) and Lawesson's reagent (210 mg, 0.50 mmol) in THF was heated at reflux for 48 h. The reaction was cooled to rt and the solvent was removed in vacuo. Chromatography of the residue (SiO2: 1-6% 2 M NH3 in MeOH/DCM) gave the title compound as an oil. MS (ESI): exact mass calcd. for C19H30N4S, 346.22; m/z found, 347.5 [M+H]+.

後処理

  1. temperatureat reflux for 48 h
  2. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-cb74db96d2e34edf8543a833a953f373
出典データセット
uspto-grants-2011_05
特許番号
US07947718B2

関連ノート

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