HCID 11794316、化合物 → HCID 9840907、化合物

HRID 1274307ノート

反応式

HRID 1274307 の反応式
[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

参加物

4

反応物 2

HCID 11794316HCID 11794316、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 9840907HCID 9840907、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-642b4d9f82614ea99aaacd4df38aeff1
出典データセット
uspto-grants-2000_12
特許番号
US06156788

反応ノート

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