Sodium borohydride → HCID 178486576、化合物

HRID 1017748

反応式

HRID 1017748 の反応式
[NH:1]1[CH:5]=[C:4]([CH:6]2[C:14]3[C:9](=[C:10]([CH3:18])[C:11]([CH3:17])=[C:12]([O:15][CH3:16])[CH:13]=3)[C:8](=[O:19])[CH2:7]2)[N:3]=[CH:2]1.[BH4-].[Na+]>C(O)C>[NH:1]1[CH:5]=[C:4]([CH:6]2[C:14]3[C:9](=[C:10]([CH3:18])[C:11]([CH3:17])=[C:12]([O:15][CH3:16])[CH:13]=3)[CH:8]([OH:19])[CH2:7]2)[N:3]=[CH:2]1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 178486575HCID 178486575、化合物

生成物 1

HCID 178486576HCID 178486576、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
37.5 °C

実験手順

3-(1H-Imidazol-4-yl)-5-methoxy-6,7-dimethylindan-1-one (0.53 g) is dissolved in ethanol (30 ml) and 0.3 g of sodium borohydride is added. The mixture is stirred at 35-40° C. for 7 hours. About 20 ml of ethanol is then distilled off and 30 ml of water is added. The solution is extracted with ethyl acetate. The combined ethyl acetate extracts are washed with water, dried with sodium sulfate, and evaporated under reduced pressure. The product is the mixture of cis- and trans-isomers (about 85:15). Crystallization of the product from ethyl acetate gives a cis-isomer, m.p. 184-189° C.

後処理

  1. distillationAbout 20 ml of ethanol is then distilled off
  2. addition30 ml of water is added
  3. extractionThe solution is extracted with ethyl acetate
  4. washThe combined ethyl acetate extracts are washed with water
  5. dry with materialdried with sodium sulfate
  6. customevaporated under reduced pressure
  7. additionthe mixture of cis- and trans-isomers (about 85:15)
  8. customCrystallization of the product from ethyl acetate
  9. customgives a cis-isomer, m.p. 184-189° C.

出典と根拠

ORDレコード
ord-a20012a5791f4dbea2b078f9a4c0951c
出典データセット
uspto-grants-2002_11
特許番号
US06479530B2

関連ノート

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