Ethanol → HCID 86691334, 화합물

HRID 881995

반응식

HRID 881995 반응식
[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]

참가 물질

4

반응물 3

HCID 702EthanolHCID 6018Tetrabenazine2회HCID 4311764Sodium borohydride

생성물 1

HCID 86691334HCID 86691334, 화합물수율 80%

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8c235ef0ec51463b8d737cf21392154f
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993766B2

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