Lawesson's reagent → HCID 18992239, 화합물

HRID 375616노트

반응식

HRID 375616 반응식
[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=O)[N:7]3[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][C:8]3=[N:9]2)=[CH:4][CH:3]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:27])=CC=1>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[S:27])[N:7]3[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][C:8]3=[N:9]2)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 139119483-Methyl-7,8,9,10-tetrahydroazepino[2,1-b]quinazolin-12(6H)-one

생성물 1

HCID 18992239HCID 18992239, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

9 g of 3-methyl-6,7,8,9,10,12-hexahydroazepino[2,1-b]quinazolin-12-one was treated with 15 g of Lawesson's reagent in toluene at reflux under nitrogen until the starting material was consumed, checked by TLC, using chloroform as eluent (24 hours). The mixture was concentrated in vacuo and chromatographed on silica gel, using chloroform as eluent. The bright yellow material was recrystallized from hexane-ethyl acetate.

후처리

  1. temperatureat reflux under nitrogen until the starting material
  2. customwas consumed
  3. custom(24 hours)
  4. concentrationThe mixture was concentrated in vacuo
  5. customchromatographed on silica gel
  6. customThe bright yellow material was recrystallized from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-154dedbd85924c5c9e7fb377657d0cc0
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05486512

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