Lawesson's reagent → 4-Morpholinobenzenecarbothioamide

HRID 56115

反応式

HRID 56115 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:15]=[CH:14][C:10]([C:11]([NH2:13])=O)=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:25])=CC=1>C1COCC1>[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:15]=[CH:14][C:10]([C:11](=[S:25])[NH2:13])=[CH:9][CH:8]=2)[CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 221422424-(Morpholin-4-yl)benzamide

生成物 1

HCID 27953604-Morpholinobenzenecarbothioamide収率 83.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

To a solution of 4-morpholinobenzamide (4.91 g, 23.80 mmol) in THF (70 mL) was added Lawesson's Reagent (10.60 g, 26.20 mmol) with stirring. The mixture was heated at 70° C. for 4 h, then cooled to rt and concentrated in vacuo. CH2Cl2 (30 mL) and water (100 mL) was added to the residue. The mixture was then filtered and the filter cake was washed with water and dried to give the title compound as a yellow solid (4.41 g, 83.3%).

後処理

  1. temperaturecooled to rt
  2. concentrationconcentrated in vacuo
  3. additionCH2Cl2 (30 mL) and water (100 mL) was added to the residue
  4. filtrationThe mixture was then filtered
  5. washthe filter cake was washed with water
  6. customdried

出典と根拠

ORDレコード
ord-b3263675a8b3462c97d4844f0524773b
出典データセット
uspto-grants-2016_09
特許番号
US09434695B2

関連ノート

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