Methanol → Fluconazole

HRID 10762

反応式

HRID 10762 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([O:22][Si](C)(C)C)([CH2:16][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1)[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1.CO.[OH-].[Na+]>O>[CH:5]1[C:6]([F:8])=[CH:7][C:2]([F:1])=[C:3]([C:9]([OH:22])([CH2:10][N:11]2[N:12]=[CH:13][N:14]=[CH:15]2)[CH2:16][N:17]2[N:18]=[CH:19][N:20]=[CH:21]2)[CH:4]=1

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 112918881,1′-[2-(2,4-Difluorophenyl)-2-[(trimethylsilyl)oxy]-1,3-propanediyl]bis[1H-1,2,4-triazole]

生成物 1

HCID 3365Fluconazole収率 87.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of 7.5 g (0.02 mol) of 2-(2,4-difluorophenyl)-1,3-bis(1,2,4-triazole-1-yl)-2-(trimethylsilyloxy)propane, 40 ml of methanol, 3 ml of water and 0.1 g of sodium hydroxide was stirred at room temperature for 1 h. After adding 300 ml of water the solution was concentrated to a volume of 50 ml with vacuum distillation. The obtained suspension was cooled to 0° C. and filtered. The obtained product was 6.12 g, water content was 11.5%. After drying at 80° C. 5.35 g of title compound was obtained. Yield: 87.4%. Mp.: 139–141° C.

後処理

  1. concentrationwas concentrated to a volume of 50 ml with vacuum distillation
  2. temperatureThe obtained suspension was cooled to 0° C.
  3. filtrationfiltered
  4. customAfter drying at 80° C

出典と根拠

ORDレコード
ord-2b91f17c041f48b492f8978539c07591
出典データセット
uspto-grants-2006_08
特許番号
US07094904B2

関連ノート

読み込み中…