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Pyridine → Allyl 3-Acetylamino-5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methylindol-4-carboxylate

HRID 52014
ノート
印刷プレビュー

反応式

HRID 52014 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([O:11][C:12]2[CH:20]=[CH:19][C:18]3[NH:17][C:16]([CH3:21])=[CH:15][C:14]=3[C:13]=2[C:22]([O:24][CH2:25][CH:26]=[CH2:27])=[O:23])[N:4]=1.[C:28]([O:31]C(=O)C)(=O)[CH3:29].[N:35]1C=CC=CC=1>>[C:28]([NH:35][C:15]1[C:14]2[C:13]([C:22]([O:24][CH2:25][CH:26]=[CH2:27])=[O:23])=[C:12]([O:11][C:5]3[N:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([O:9][CH3:10])[N:6]=3)[CH:20]=[CH:19][C:18]=2[NH:17][C:16]=1[CH3:21])(=[O:31])[CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 19962801Allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methylindol-4-carboxylate

生成物 1

HCID 19962751Allyl 3-Acetylamino-5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methylindol-4-carboxylate収率 87%

実験手順

0.5 g of allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methylindol-4-carboxylate was dissolved in 10 ml of pyridine, and 0.16 g of acetic anhydride was added thereto. The mixture was stirred for 12 hours. The reaction solution was poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous magnesium sulfate. The residue obtained by concentration under reduced pressure, was crystallized with isopropyl ether to obtain 0.49 g (yield: 87%) of the desired compound. mp: 177°-180° C.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe residue obtained by concentration under reduced pressure
  5. customwas crystallized with isopropyl ether

出典と根拠

ORDレコード
ord-a27712b0f6a2409f9d9fe02c132d3342
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05616537

反応ノート

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