HCID 11794316, 화합물 → HCID 9840907, 화합물

HRID 1274307노트

반응식

HRID 1274307 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[C:9]([S:22][C:23]2[CH:33]=[CH:32][C:26]([C:27](OCC)=[O:28])=[CH:25][CH:24]=2)=[CH:10][C:11]2[C:12]([CH3:21])([CH3:20])[CH2:13][CH2:14][C:15]([CH3:19])([CH3:18])[C:16]=2[CH:17]=1>C1COCC1>[CH3:7][C:8]1[C:9]([S:22][C:23]2[CH:33]=[CH:32][C:26]([CH2:27][OH:28])=[CH:25][CH:24]=2)=[CH:10][C:11]2[C:12]([CH3:21])([CH3:20])[CH2:13][CH2:14][C:15]([CH3:18])([CH3:19])[C:16]=2[CH:17]=1

참가 물질

4

반응물 2

HCID 11794316HCID 11794316, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 9840907HCID 9840907, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

144 mg (3.8 mmol) of lithium aluminum hydride and 50 ml of THF were introduced into a three-necked flask and under a nitrogen stream. Next, a solution of 1.4 g (3.8 mmol) of ethyl 4-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-2-naphthylthio)benzoate in 25 ml of THF was introduced dropwise and the mixture was heated at reflux for 8 hours. The excess hydride was destroyed with a potassium sodium tartrate solution and the reaction medium was extracted with ethyl acetate. The organic phase was decanted off, dried over magnesium sulfate and evaporated.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 8 hours
  3. customThe excess hydride was destroyed with a potassium sodium tartrate solution
  4. extractionthe reaction medium was extracted with ethyl acetate
  5. customThe organic phase was decanted off
  6. dry with materialdried over magnesium sulfate
  7. customevaporated

출처 및 근거

ORD 기록
ord-642b4d9f82614ea99aaacd4df38aeff1
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06156788

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