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Sodium borohydride → 1-[8-Fluoro-2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-9-yl]ethanol

HRID 1530703
ノート
印刷プレビュー

反応式

HRID 1530703 の反応式
[BH4-].[Na+].[F:3][C:4]1[CH:5]=[C:6]2[C:15](=[CH:16][C:17]=1[C:18](=[O:20])[CH3:19])[C:14]1[N:10]([CH:11]=[C:12]([C:21]3[N:25]([CH:26]([CH3:28])[CH3:27])[N:24]=[C:23]([CH3:29])[N:22]=3)[N:13]=1)[CH2:9][CH2:8][O:7]2>CO>[F:3][C:4]1[CH:5]=[C:6]2[C:15](=[CH:16][C:17]=1[CH:18]([OH:20])[CH3:19])[C:14]1[N:10]([CH:11]=[C:12]([C:21]3[N:25]([CH:26]([CH3:28])[CH3:27])[N:24]=[C:23]([CH3:29])[N:22]=3)[N:13]=1)[CH2:9][CH2:8][O:7]2
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 2

HCID 4311764Sodium borohydrideHCID 683130591-{12-Fluoro-4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaen-13-yl}ethan-1-one

生成物 1

HCID 683128551-[8-Fluoro-2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-9-yl]ethanol収率 96.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a stirred suspension of NaBH4 (638 mg, 16.8 mmol) in MeOH (15 mL), was added a solution of 1-{12-fluoro-4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaen-13-yl}ethan-1-one (1.55 g, 4.20 mmol) in MeOH (15 mL) at 0° C. under a nitrogen atmosphere. After the addition was completed, the cooling bath was removed and the mixture was stirred at room temperature for 1 h. After removal of the solvent, the residue was purified by silica gel chromatography using 5% dichloromethane in methanol as eluant to give the title compound (1.5 g, 96% yield) as a white solid. LCMS m/z [M+H]+ 372.1

後処理

  1. additionAfter the addition
  2. customthe cooling bath was removed
  3. customAfter removal of the solvent
  4. customthe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-01f4631a61a84b73b091bae59eda5e63
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090628B2

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