Pyridine → HCID 178487221、化合物

HRID 2165149ノート

反応式

HRID 2165149 の反応式
N1C=CC=CC=1.[CH3:7][S:8](Cl)(=[O:10])=[O:9].[CH3:12][O:13][C:14]1[CH:15]=[CH:16][C:17]2[CH:20]=[C:19]([CH2:21][OH:22])[C:18]=2[CH:23]=1>ClCCl>[CH3:12][O:13][C:14]1[CH:15]=[CH:16][C:17]2[CH:20]=[C:19]([CH2:21][O:22][S:8]([CH3:7])(=[O:10])=[O:9])[C:18]=2[CH:23]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 23044250HCID 23044250、化合物

生成物 1

HCID 178487221HCID 178487221、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

6.1 ml (76 mmol) of pyridine and 3.6 ml (46 mmol) of methanesulphonic acid chloride are added at 0° C., while stirring, with the exclusion of moisture, to 5.0 g (30.5 mmol) of (5-methoxybenzocyclobuten-1-yl)methanol in 50 ml of dichloromethane. The mixture is then stirred at room temperature for a further 18 hours to complete the reaction. 50 ml of ice-water are then added and the whole is stirred for 30 minutes. The organic phase is separated off, washed once in each case with 2N sodium hydroxide solution, 2N hydrochloric acid and water, dried over sodium sulphate and concentrated under reduced pressure. Methanesulphonic acid (5-methoxybenzocyclobuten-1-ylmethyl) ester is obtained in the form of a viscous oil, Rf=0.4, toluene/ethyl acetate (9:1).

後処理

  1. customthe reaction
  2. stirringthe whole is stirred for 30 minutes
  3. customThe organic phase is separated off
  4. washwashed once in each case with 2N sodium hydroxide solution, 2N hydrochloric acid and water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-69970ee26a5d4be0bf1a2fce2bdb40d8
出典データセット
uspto-grants-1990_07
特許番号
US04939160

反応ノート

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