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

HRID 398821ノート

反応式

HRID 398821 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6386tert-Butanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-b138a27a123e467da2a8f5b77082f856
出典データセット
uspto-grants-1998_10
特許番号
US05817652

反応ノート

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