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Ammonium Chloride → HCID 22648514、化合物

HRID 393118
ノート
印刷プレビュー

反応式

HRID 393118 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].C([O:9][C:10](=O)[CH2:11][C:12]([S:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)([CH3:16])[CH2:13][CH2:14][CH3:15])C.[NH4+].[Cl-]>CCOCC>[CH2:18]([S:17][C:12]([CH3:16])([CH2:13][CH2:14][CH3:15])[CH2:11][CH2:10][OH:9])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 21226445Aluminium lithium hydrideHCID 53885188HCID 53885188、化合物

生成物 1

HCID 22648514HCID 22648514、化合物収率 95.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

At a temperature of 0° C. to a suspension of 6.8 g (0.18 mol) of LiAlH4 in 200 ml of Et2O was slowly added 50.0 g (0.18 mol) of (rac)-3-benzylsulfanyl-3-methyl-hexanoic acid ethyl ester of step (b) under stirring such that the temperature did not exceed 10° C. Stirring was continued for 1 h and under cooling acetone and then 400 ml of a saturated NH4Cl solution was slowly added. The reaction mixture was extracted three times with 200 ml of Et2O, the combined organic layers were dried over Na2SO4 and concentrated in vacuo and gave 40.8 g of a yellowish oil. After drying in high vacuo (0.05 mbar/150° C.) 32.5 g (75%) of (rac)-3-benzylsulfanyl-3-methyl-hexan-1-ol in the form of a yellowish oil was obtained.

後処理

  1. customdid not exceed 10° C
  2. stirringStirring
  3. extractionThe reaction mixture was extracted three times with 200 ml of Et2O
  4. dry with materialthe combined organic layers were dried over Na2SO4
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b6a18d1a9bf342fa8226c3cd0a7bf831
出典データセット
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06805893B2

反応ノート

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