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Acetic Acid → 1-Benzylpiperidine-4-thiol

HRID 1742629
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HRID 1742629 반응식
N=C1N(CC[S:9][CH:10]2[CH2:15][CH2:14][N:13]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:12][CH2:11]2)C2C=CC(OC(F)(F)F)=CC=2S1.C(N1CCC(SC(=O)C)CC1)C1C=CC=CC=1.C(O)(=O)C.S([O-])([O-])(=O)=O.[NH4+].[NH4+]>[OH-].[Na+]>[CH2:16]([N:13]1[CH2:14][CH2:15][CH:10]([SH:9])[CH2:11][CH2:12]1)[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1
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참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 6097028Ammonium SulfateHCID 151664202-Imino-3-{2-[(1-benzyl-4-piperidyl)thio]ethyl}-6-trifluoromethoxybenzothiazolineHCID 151664211-Benzyl-4-acetylthiopiperidine

생성물 1

HCID 112757831-Benzylpiperidine-4-thiol

시약·촉매·용매 1

HCID 14798
Sodium Hydroxide
용매

실험 절차

The 1-benzyl-4-mercaptopiperidine may be prepared in the following manner: 8 g of 1-benzyl-4-acetylthiopiperidine dissolved in 85 cm3 of a 6% aqueous solution of sodium hydroxide are stirred under a nitrogen stream for 16 hours. 10 cm3 of acetic acid and 57.5 g of ammonium sulphate are added to this solution. The mixture is then extracted with two times 100 cm3 of diethyl ether and the organic phase is dried over anhydrous magnesium sulphate and concentrated to dryness at 40° C. under reduced pressure (20 mm of mercury; 2.7 kPa). 5.5 g of 1-benzyl-4-mercaptopiperidine are thus directly isolated in the form of an oil which is used as it is in subsequent synthesis.

후처리

  1. extractionThe mixture is then extracted with two times 100 cm3 of diethyl ether
  2. dry with materialthe organic phase is dried over anhydrous magnesium sulphate
  3. concentrationconcentrated to dryness at 40° C. under reduced pressure (20 mm of mercury; 2.7 kPa)

출처 및 근거

ORD 기록
ord-4cb5f25197e24a0bb27ecf95c4cf1cb1
출처 데이터셋
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05340824

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