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Ammonium Chloride → HCID 22648514, 화합물

HRID 393118
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HRID 393118 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 21226445Aluminium lithium hydrideHCID 53885188HCID 53885188, 화합물

생성물 1

HCID 22648514HCID 22648514, 화합물수율 95.1%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b6a18d1a9bf342fa8226c3cd0a7bf831
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06805893B2

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