Sodium Chloride → 1-[4-(Tributylstannyl)-3,6-dihydropyridin-1(2H)-yl]ethan-1-one

HRID 2184801ノート

反応式

HRID 2184801 の反応式
S(Cl)(C)(=O)=O.[C:6]([N:9]1[CH2:14][CH2:13][C:12](O)([Sn:15]([CH2:24][CH2:25][CH2:26][CH3:27])([CH2:20][CH2:21][CH2:22][CH3:23])[CH2:16][CH2:17][CH2:18][CH3:19])[CH2:11][CH2:10]1)(=[O:8])[CH3:7].C(N(CC)CC)C.[Na+].[Cl-]>ClCCl>[C:6]([N:9]1[CH2:10][CH:11]=[C:12]([Sn:15]([CH2:24][CH2:25][CH2:26][CH3:27])([CH2:16][CH2:17][CH2:18][CH3:19])[CH2:20][CH2:21][CH2:22][CH3:23])[CH2:13][CH2:14]1)(=[O:8])[CH3:7]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 156368991-Acetyl-4-hydroxy-4-tributylstannyl-piperidine

生成物 1

HCID 156368961-[4-(Tributylstannyl)-3,6-dihydropyridin-1(2H)-yl]ethan-1-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Under an inert atmosphere, 1.3 equivalents of mesyl chloride in 15 ml of dichloromethane are added dropwise to a solution of 0.16 mmol of the compound obtained in Step A and 2.8 equivalents of triethylamine in 1 litre of dichloromethane at 0° C. After stirring the mixture at ambient temperature for 4 days, a saturated aqueous solution of NaCl is added. After extraction, drying, filtration and concentration of the organic phase under reduced pressure, chromatography of the residue on silica gel (dichloromethane/ethanol: 97/3) enables the expected product to be isolated.

後処理

  1. extractionAfter extraction
  2. customdrying
  3. filtrationfiltration and concentration of the organic phase under reduced pressure, chromatography of the residue on silica gel (dichloromethane/ethanol: 97/3)
  4. customto be isolated

出典と根拠

ORDレコード
ord-19a6dbc2aa70430ab76a3347e312fc3d
出典データセット
uspto-grants-2002_06
特許番号
US06399616B1

反応ノート

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