Lawesson's reagent → 4-Morpholinobenzenecarbothioamide

HRID 56115

반응식

HRID 56115 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 27953604-Morpholinobenzenecarbothioamide수율 83.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
70 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-b3263675a8b3462c97d4844f0524773b
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434695B2

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