Lawesson's reagent → Ammonia

HRID 30487

反応式

HRID 30487 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-40d0cb1381bc469c859c24aedd943567
出典データセット
uspto-grants-2008_09
特許番号
US07423147B2

関連ノート

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