Lawesson's reagent → HCID 18992239、化合物

HRID 375616ノート

反応式

HRID 375616 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 18992239HCID 18992239、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-154dedbd85924c5c9e7fb377657d0cc0
出典データセット
uspto-grants-1996_01
特許番号
US05486512

反応ノート

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