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Water → HCID 19756351、化合物

HRID 1587830
ノート
印刷プレビュー

反応式

HRID 1587830 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][CH2:9][CH2:10][O:11][Si:12]([C:25]([CH3:28])([CH3:27])[CH3:26])([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:6][CH:7]=1.[C:29]([CH2:33][C:34](OC)=[O:35])(=O)[CH2:30][CH3:31].C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1C=CC=CC=1>[Si:12]([O:11][CH2:10][CH2:9][O:8][C:5]1[N:6]=[C:7]2[C:2](=[CH:3][CH:4]=1)[NH:1][C:29]([CH2:30][CH3:31])=[CH:33][C:34]2=[O:35])([C:25]([CH3:28])([CH3:27])[CH3:26])([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=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 6101p-Toluenesulfonic acidHCID 121699Methyl 3-oxovalerateHCID 19756412HCID 19756412、化合物

生成物 1

HCID 19756351HCID 19756351、化合物収率 62%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of compound C (10 g), methyl propionylacetate (11.5 g) and p-toluenesulphonic acid (0.1 g) in benzene (40 ml) was heated under reflux with azeotropic removal of water for 20 hours. Volatile material was removed by evaporation and the residue added to a refluxing eutectic mixture of 26.5% v/v diphenyl and 73.5% v/v diphenyl oxide (30 ml). The solution was heated under reflux for 1 hour, cooled and diluted with hexane (100 ml). The precipitated solid was filtered off and triturated with hot methanol (100 ml) to give 2-ethyl-6-[2-(trimethylsilyl)ethoxy]-1,5-naphthyridin-4-(1H)-one (D) (in 62% yield) as a white solid, m.p. 193° C.; NMR: -0.1(s,9H), 0.85(t,2H), 1.3(t,3H), 2.8(q,2H), 4.1(t,2H), 6.55(s,1H), 6.9(d,1H), 8.2(d,1H).

後処理

  1. customVolatile material was removed by evaporation
  2. additionthe residue added to a refluxing eutectic mixture of 26.5% v/v diphenyl and 73.5% v/v diphenyl oxide (30 ml)
  3. temperatureThe solution was heated
  4. temperatureunder reflux for 1 hour
  5. temperaturecooled
  6. additiondiluted with hexane (100 ml)
  7. filtrationThe precipitated solid was filtered off
  8. customtriturated with hot methanol (100 ml)

出典と根拠

ORDレコード
ord-5b75ffbc2bad442695fc930bfec7e133
出典データセット
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05219863

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