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Dimethylformamide → HCID 13175316、化合物

HRID 2418216
ノート
印刷プレビュー

反応式

HRID 2418216 の反応式
CN(C)C=O.Cl[C:7]([O:9][CH2:10][CH3:11])=[O:8].[O:12]=[C:13]1[N:18]2[C:19]3[C:24]([NH:25][CH2:26][C:17]2=[N:16][CH:15]=[C:14]1[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:23][CH:22]=[CH:21][CH:20]=3>O>[O:12]=[C:13]1[N:18]2[C:19]3[C:24]([N:25]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:26][C:17]2=[N:16][CH:15]=[C:14]1[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:23][CH:22]=[CH:21][CH:20]=3
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 6228DimethylformamideHCID 10928Ethyl chloroformateHCID 13175315HCID 13175315、化合物

生成物 1

HCID 13175316HCID 13175316、化合物収率 41%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4 ml of dry dimethylformamide were saturated with nitrogen for 10 minutes before 150 mg of ethyl chloroformate and 280 mg of ethyl 5,6-dihydro-1-oxo-1H-pyrimido [1,2-a] quinoxaline-2-carboxylate were added thereto. The solution obtained was left at room temperature overnight and then was poured into water. The mixture was extracted with ethyl acetate and the organic phase was dried over MgSO4 and evaporated to dryness. The residue was chromatographed over silica gel and eluted with ethyl acetate to obtain 140 mg (41% yield) of diethyl 5,6-dihydro-1-oxo-1H-pyrimido [1,2-a] quinoxaline-2,6-dicarboxylate melting at 140°-2° C.

後処理

  1. additionwere added
  2. customThe solution obtained
  3. extractionThe mixture was extracted with ethyl acetate
  4. dry with materialthe organic phase was dried over MgSO4
  5. customevaporated to dryness
  6. customThe residue was chromatographed over silica gel
  7. washeluted with ethyl acetate

出典と根拠

ORDレコード
ord-a24dfdf9a5314ed18eb735361453d567
出典データセット
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04472401

反応ノート

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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