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Acetic Acid → 1-Benzylpiperidine-4-thiol

HRID 1742629
ノート
印刷プレビュー

反応式

HRID 1742629 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 112757831-Benzylpiperidine-4-thiol

試薬・触媒・溶媒 1

HCID 14798
Sodium Hydroxide
溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-4cb5f25197e24a0bb27ecf95c4cf1cb1
出典データセット
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05340824

反応ノート

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