Lawesson's reagent → Ammonia

HRID 551597

반응식

HRID 551597 반응식
[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]

참가 물질

5

반응물 2

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

생성물 2

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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]+.

후처리

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

출처 및 근거

ORD 기록
ord-cb74db96d2e34edf8543a833a953f373
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947718B2

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