Lawesson's reagent → HCID 57650584、化合物

HRID 2063475ノート

反応式

HRID 2063475 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([NH:10][C:11]([C@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=O)[CH3:9])=[CH:4][CH:3]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:34])=CC=1>C1(C)C=CC=CC=1.CCOC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([NH:10][C:11]([C@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[S:34])[CH3:9])=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 87949Lawesson's reagentHCID 51968676HCID 51968676、化合物

生成物 1

HCID 57650584HCID 57650584、化合物収率 140.3%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture the product of Step A (3 g, 8.5 mmol) and Lawesson's reagent (1.7 g, 4.25 mmol) in toluene (100 ml) was refluxed for 2 h. The mixture was cooled to room temperature and then was diluted with EtOAc (100 ml), washed with 1N NaOH (2×50 ml), dried over Na2SO4, and concentrated in vacuo. Flash chromatography purification (DCM/MeOH gradient, 0-15% MeOH) provided the desired product as a white solid (2.2 g, 71%)

後処理

  1. washwashed with 1N NaOH (2×50 ml)
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customFlash chromatography purification (DCM/MeOH gradient, 0-15% MeOH)

出典と根拠

ORDレコード
ord-ca4068071ae64372bd408429d756ddfd
出典データセット
uspto-grants-2012_10
特許番号
US08288371B2

反応ノート

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