Potassium → (+/-)-3-Butyl-3-ethyl-2,3-dihydro-1,4-benzothiazepine

HRID 398821노트

반응식

HRID 398821 반응식
[CH2:1]([C:5]1([CH2:16][CH3:17])[NH:11][CH2:10][C:9]2[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=2[S:7][CH2:6]1)[CH2:2][CH2:3][CH3:4].[K]>C(O)(C)(C)C.O>[CH2:1]([C:5]1([CH2:16][CH3:17])[N:11]=[CH:10][C:9]2[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=2[S:7][CH2:6]1)[CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 2

HCID 5462222PotassiumHCID 18968854(+/-)-3-Butyl-3-ethyl-2,3,4,5-tetrahydro-1,4-benzothiazepine

생성물 1

HCID 18968787(+/-)-3-Butyl-3-ethyl-2,3-dihydro-1,4-benzothiazepine수율 99.1%

시약·촉매·용매 2

HCID 962Water용매HCID 6386tert-Butanol용매

실험 절차

To a solution of the product from step (b) (6.0 g) in tert-butyl alcohol (180 ml) was added a solution of potassium permangante (5.7 g) in water (90 ml). The mixture was heated to reflux for 10 minutes, cooled to room temperature, and filtered through celite. Solvent was evaporated to provide the title compound (5.9 g) as a colorless oil. 1H NMR consistent with the proposed structure.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 10 minutes
  3. filtrationfiltered through celite
  4. customSolvent was evaporated

출처 및 근거

ORD 기록
ord-b138a27a123e467da2a8f5b77082f856
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05817652

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