ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → 6-[(6,7-Dimethoxy-4-quinolyl)oxy]-1,4-dihydro-2H-3,1-benzoxazin-2-one

HRID 228535
ノート
印刷プレビュー

反応式

HRID 228535 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:9]2[C:18]3[C:13](=[CH:14][C:15]([O:21][CH3:22])=[C:16]([O:19][CH3:20])[CH:17]=3)[N:12]=[CH:11][CH:10]=2)=[CH:4][C:3]=1[CH2:23][OH:24].Cl[C:26](Cl)([O:28]C(=O)OC(Cl)(Cl)Cl)Cl.O>C(N(CC)CC)C.C1(C)C=CC=CC=1>[CH3:20][O:19][C:16]1[CH:17]=[C:18]2[C:13](=[CH:14][C:15]=1[O:21][CH3:22])[N:12]=[CH:11][CH:10]=[C:9]2[O:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:26](=[O:28])[O:24][CH2:23][C:3]=2[CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 94429TriphosgeneHCID 68830546{2-Amino-5-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}methanol

生成物 1

HCID 231564336-[(6,7-Dimethoxy-4-quinolyl)oxy]-1,4-dihydro-2H-3,1-benzoxazin-2-one収率 39%

試薬・触媒・溶媒 1

HCID 22504574Toluene triethylamine溶媒

実験手順

{2-Amino-5-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}methanol (63 mg) was dissolved in heated triethylamine/toluene (1.2 ml/6 ml) to prepare a solution. Triphosgene (98 mg) was added to the solution and was heated under reflux for 2 min. The reaction solution was cooled to room temperature, water was then added to the reaction solution, and the mixture was extracted with chloroform. The chloroform layer was then washed with water and saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by column chromatography on silica gel using acetone-chloroform to give the title compound (24 mg, yield 39%).

後処理

  1. customto prepare a solution
  2. temperaturewas heated
  3. temperatureunder reflux for 2 min
  4. extractionthe mixture was extracted with chloroform
  5. washThe chloroform layer was then washed with water and saturated brine
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. customThe solvent was removed
  8. distillationby distillation under the reduced pressure
  9. customthe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-f33e7705410f4bfdb218846039397b48
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07560558B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート