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Benzyl mercaptan → 2-Benzylsulfanyl-5-(1-methanesulfonyl-piperidin-4-yloxy)-pyridine

HRID 1049042
ノート
印刷プレビュー

反応式

HRID 1049042 の反応式
[H-].[Na+].[CH2:3]([SH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl[C:12]1[CH:17]=[CH:16][C:15]([O:18][CH:19]2[CH2:24][CH2:23][N:22]([S:25]([CH3:28])(=[O:27])=[O:26])[CH2:21][CH2:20]2)=[CH:14][N:13]=1>CN(C=O)C.CCOC(C)=O>[CH2:3]([S:10][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH:19]2[CH2:24][CH2:23][N:22]([S:25]([CH3:28])(=[O:26])=[O:27])[CH2:21][CH2:20]2)=[CH:14][N:13]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=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 3

HCID 7509Benzyl mercaptanHCID 24758Sodium hydrideHCID 867218872-Chloro-5-(1-methanesulfonyl-piperidin-4-yloxy)-pyridine

生成物 1

HCID 867218882-Benzylsulfanyl-5-(1-methanesulfonyl-piperidin-4-yloxy)-pyridine収率 51%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

A suspension of NaH (60% dispersion in mineral oil, 413 mg, 10.32 mmol) in dry DMF (12 mL) at 0° C. was treated dropwise with benzyl mercaptan (1.21 mL, 10.32 mmol). After the addition the mixture was stirred at room temperature for 15 minutes. 2-Chloro-5-(1-methanesulfonyl-piperidin-4-yloxy)-pyridine (1.00 g, 3.44 mmol) was added and the mixture stirred at room temperature for 18 hours, heated at 80° C. for a further 8 hours and allowed to cool overnight. The mixture was diluted with EtOAc, washed with water and brine, dried over Na2SO4 and concentrated under vacuum. Purified by silica gel column chromatography (30-50% EtOAc in cyclohexane) to give 2-benzylsulfanyl-5-(1-methanesulfonyl-piperidin-4-yloxy)-pyridine (659 mg, 51%). 1H NMR (300 MHz, CDCl3) δ 8.20 (br s, 1H), 7.40-7.34 (m, 2H), 7.32-7.18 (s, 4H), 7.14-7.05 (m, 2H), 4.52-4.43 (m, 1H), 4.39 (s, 2H), 3.36 (t, J=5.6 Hz, 4H), 2.82 (s, 3H), 2.08-1.91 (m, 4H). LCMS (m/z, Method A) ES+ 379.1 [M+1]+.

後処理

  1. additionAfter the addition the mixture
  2. stirringthe mixture stirred at room temperature for 18 hours
  3. temperatureheated at 80° C. for a further 8 hours
  4. temperatureto cool overnight
  5. washwashed with water and brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under vacuum
  8. customPurified by silica gel column chromatography (30-50% EtOAc in cyclohexane)

出典と根拠

ORDレコード
ord-2371bc3f757a42f9a780561db7ec7f32
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09382222B2

反応ノート

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