Water → HCID 13505933、化合物

HRID 279776ノート

反応式

HRID 279776 の反応式
[CH2:1]([O:3][C:4]([C:6]1(C(OCC)=O)[CH2:9][C:8](=[O:10])[N:7]1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][C:13]=1[O:20][CH3:21])=[O:5])[CH3:2].[Cl-].[Na+].O>CS(C)=O>[CH2:1]([O:3][C:4]([CH:6]1[CH2:9][C:8](=[O:10])[N:7]1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][C:13]=1[O:20][CH3:21])=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 962WaterHCID 5234Sodium Chloride2 回HCID 13505928HCID 13505928、化合物

生成物 1

HCID 13505933HCID 13505933、化合物収率 90.2%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture of 66.2 g (0.18 mole) of diethyl[1-(2,4-dimethoxy-benzyl)-4-oxo-2,2-azetidine-dicarboxylate] prepared according to the preceding paragraph, 70 ml of dimethyl sulfoxide, 12.7 g (0.22 mole) of sodium chloride and 6.5 ml (0.36 mole) of water is stirred on an oil bath (temperature 170°-180° C. for 6 hours. The reaction mixture is poured into 500 ml of a saturated aqueous sodium chloride solution, extracted five times with 100 ml ethyl acetate each, the organic phase is dried over anhydrous magnesium sulfate, filtered and from the filtrate the ethyl acetate is distilled off. Thus 47.6 g of ethyl-[1-(2,4-dimethoxy-benzyl)-4-oxo-2-azetidine-carboxylate] are obtained. B.p.: 170°-176° C./0.15 Hgmm.

後処理

  1. customprepared
  2. extractionextracted five times with 100 ml ethyl acetate each, the organic phase
  3. dry with materialis dried over anhydrous magnesium sulfate
  4. filtrationfiltered and from the filtrate the ethyl acetate
  5. distillationis distilled off

出典と根拠

ORDレコード
ord-86aea116717242f48f5b6611ddc0bf3e
出典データセット
uspto-grants-1986_05
特許番号
US04587049

反応ノート

読み込み中…