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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
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Water → HCID 67716628、化合物

HRID 266161
ノート
印刷プレビュー

反応式

HRID 266161 の反応式
[H-].[Na+].[C:3]1([NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl[CH2:17][C:18]1[N:27]=[C:26]([C:28]2[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[C:30]([O:36][CH3:37])[CH:29]=2)[C:25]2[C:20](=[CH:21][C:22]([O:40][CH3:41])=[C:23]([O:38][CH3:39])[CH:24]=2)[N:19]=1.O>CN(C)C=O>[C:10]1([N:9]([CH2:17][C:18]2[N:27]=[C:26]([C:28]3[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[C:30]([O:36][CH3:37])[CH:29]=3)[C:25]3[C:20](=[CH:21][C:22]([O:40][CH3:41])=[C:23]([O:38][CH3:39])[CH:24]=3)[N:19]=2)[C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 11487DiphenylamineHCID 24758Sodium hydrideHCID 107856562-Chloromethyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline

生成物 1

HCID 67716628HCID 67716628、化合物収率 20%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

Sodium hydride (oily, 60%, 0.129 g) was added to a solution of diphenylamine (0.497 g) in N,N-dimethylformamide (10 ml), and the mixture was stirred at room temperature for 20 minutes. Then, 2-chloromethyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline (1.0 g) was added, and the mixture was stirred at 100° C. for 4 hours. The reaction mixture was poured into water, and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions eluted with ethyl acetate - hexane (1:1, v/v) gave 2-(N,N-diphenylaminomethyl)-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline (0.27 g, 20%). This compound was recrystallized from ethyl acetate - hexane. Colorless prisms, mp. 215°-216° C.

後処理

  1. stirringthe mixture was stirred at 100° C. for 4 hours
  2. extractionextracted with ethyl acetate
  3. washThe ethyl acetate layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. washThe fractions eluted with ethyl acetate - hexane (1:1

出典と根拠

ORDレコード
ord-806c2db3d48a413db6eb0ab188b8fe40
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05650410

反応ノート

読み込み中…

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