Ethanol → HCID 86691334、化合物

HRID 881995

反応式

HRID 881995 の反応式
[CH3:1][CH:2]([CH2:4][CH:5]1[C:18](=[O:19])[CH2:17][CH:16]2[N:7]([CH2:8][CH2:9][C:10]3[C:15]2=[CH:14][C:13]([O:20][CH3:21])=[C:12]([O:22][CH3:23])[CH:11]=3)[CH2:6]1)C.[BH4-].[Na+].[CH2:26]([OH:28])C>>[OH:19][CH:18]1[CH2:17][CH:16]2[N:7]([CH2:8][CH2:9][C:10]3[CH:11]=[C:12]([O:22][CH3:23])[C:13]([O:20][CH3:21])=[CH:14][C:15]=32)[CH2:6][CH:5]1[CH2:4][CH:2]([O:28][CH3:26])[CH3:1]

参加物

4

反応物 3

HCID 702EthanolHCID 6018Tetrabenazine2 回HCID 4311764Sodium borohydride

生成物 1

HCID 86691334HCID 86691334、化合物収率 80%

反応条件

温度
0 °C

実験手順

Tetrabenazine (Formula 1; 9.01 mg, 0.0284 mmol) was dissolved in 1 mL of ethanol, the solution was cooled to 0° C., and then NaBH4 (3.22 mg, 0.0851 mmol) was slowly added thereto. The temperature was heated to normal temperature and then the mixture was stirred for 1 hr. The mixture was distilled under reduced pressure, water (3 mL) and CH2Cl2 (3 mL) were added thereto to extract an organic layer, and the organic layer collected was washed with a saturated K2CO3 aqueous solution. Anhydrous magnesium sulfate was used to dry the organic layer, filtration under reduced pressure and evaporation under reduced pressure were performed, and then column chromatography was used to obtain 7.30 mg (yield 80%) of the title compound.

後処理

  1. temperatureThe temperature was heated to normal temperature
  2. distillationThe mixture was distilled under reduced pressure, water (3 mL) and CH2Cl2 (3 mL)
  3. additionwere added
  4. extractionto extract an organic layer
  5. customthe organic layer collected
  6. washwas washed with a saturated K2CO3 aqueous solution
  7. customto dry
  8. filtrationthe organic layer, filtration
  9. customunder reduced pressure and evaporation under reduced pressure

出典と根拠

ORDレコード
ord-8c235ef0ec51463b8d737cf21392154f
出典データセット
uspto-grants-2015_03
特許番号
US08993766B2

関連ノート

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