Sodium borohydride → 2-hydroxymethylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one

HRID 1281886ノート

反応式

HRID 1281886 の反応式
[CH:1]([C:3]1[S:17][C:6]2[O:7][C:8]3[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=3[NH:10][C:11](=[O:12])[C:5]=2[CH:4]=1)=[O:2].[BH4-].[Na+]>CO.O>[OH:2][CH2:1][C:3]1[S:17][C:6]2[O:7][C:8]3[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=3[NH:10][C:11](=[O:12])[C:5]=2[CH:4]=1

参加物

5

反応物 2

HCID 4311764Sodium borohydrideHCID 184221402-Formylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one

生成物 1

HCID 184221522-hydroxymethylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one収率 62%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

2-Formylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.6 g) was suspended in methanol (30 ml) and sodium borohydride (480 mg) was added. The mixture was stirred at room temperature for 1.5 hours. The reaction mixture was diluted with water and extracted 3 times with chloroform. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. To the residue were added chloroform and diisopropyl ether and the precipitated crystals were collected by filtration to give 2-hydroxymethylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.0 g).

後処理

  1. extractionextracted 3 times with chloroform
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. additionTo the residue were added chloroform and diisopropyl ether
  5. filtrationthe precipitated crystals were collected by filtration

出典と根拠

ORDレコード
ord-bbae3245b4314f84ae17d176b46eac19
出典データセット
uspto-grants-2002_09
特許番号
US06455521B1

反応ノート

読み込み中…