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Methanol → 3-[1-(6,7-Dimethoxy-4-quinazolinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-6-(1-hydroxyethyl)-1-methyl-2,4-dioxoquinazoline

HRID 55053
ノート
印刷プレビュー

反応式

HRID 55053 の反応式
CO.C(Cl)(Cl)Cl.[C:7]([C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][CH:19]=1)[N:16]([CH3:20])[C:15](=[O:21])[N:14]([CH:22]1[CH2:27][CH2:26][N:25]([C:28]3[C:37]4[C:32](=[CH:33][C:34]([O:40][CH3:41])=[C:35]([O:38][CH3:39])[CH:36]=4)[N:31]=[CH:30][N:29]=3)[CH2:24][CH2:23]1)[C:13]2=[O:42])(=[O:9])[CH3:8].[BH4-].[Na+]>O>[CH3:39][O:38][C:35]1[CH:36]=[C:37]2[C:32](=[CH:33][C:34]=1[O:40][CH3:41])[N:31]=[CH:30][N:29]=[C:28]2[N:25]1[CH2:26][CH2:27][CH:22]([N:14]2[C:13](=[O:42])[C:12]3[C:17](=[CH:18][CH:19]=[C:10]([CH:7]([OH:9])[CH3:8])[CH:11]=3)[N:16]([CH3:20])[C:15]2=[O:21])[CH2:23][CH2:24]1
参加物反応条件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 887MethanolHCID 6212ChloroformHCID 4311764Sodium borohydrideHCID 229233736-Acetyl-3-[1-(6,7-dimethoxy-4-quinazolinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-1-methyl-2,4-dioxo-quinazoline

生成物 1

HCID 229235413-[1-(6,7-Dimethoxy-4-quinazolinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-6-(1-hydroxyethyl)-1-methyl-2,4-dioxoquinazoline収率 73%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

In a solvent mixture of 3ml of methanol and 3 ml of chloroform was dissolved 200.0 mg (0.41 mmol) of Compound 63 obtained in Example 50, and sodium borohydride was added thereto in excess, followed by heating at 60° C. for 30 minutes. After cooling, water was added to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was washed and dried, and the solvent was distilled off under reduced pressure. To the residue was added ether, and the precipitated crystals were collected by filtration and dried to give 146.4 mg (yield: 73%) of Compound 60 as white crystals.

後処理

  1. additionwas added
  2. temperatureAfter cooling
  3. extractionthe mixture was extracted with chloroform
  4. washThe organic layer was washed
  5. customdried
  6. distillationthe solvent was distilled off under reduced pressure
  7. additionTo the residue was added ether
  8. filtrationthe precipitated crystals were collected by filtration
  9. customdried

出典と根拠

ORDレコード
ord-981fd36074be42f48834c14061dea498
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05624926

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート