Hydrochloric Acid → HCID 14456866、化合物

HRID 279780ノート

反応式

HRID 279780 の反応式
[CH3:1][O:2][C:3]1[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[CH:16][C:4]=1[CH2:5][N:6]1[C:9](=[O:10])[CH2:8][CH:7]1[C:11](OCC)=[O:12].Cl>CO>[CH3:1][O:2][C:3]1[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[CH:16][C:4]=1[CH2:5][N:6]1[CH:7]([CH2:11][OH:12])[CH2:8][C:9]1=[O:10]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 13505933HCID 13505933、化合物

生成物 1

HCID 14456866HCID 14456866、化合物収率 96.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

47.6 g (0.162 mole) of ethyl 1-(2,4-dimethoxybenzyl)-4-oxo-2-azetidine-carboxylate prepared according to paragraph e) of Example 1 are reacted with 12.4 g (0.327 moles) of sodium-[tetrahydro-borate(III)] in 200 ml of methanol under external ice-cooling. The reaction takes place within about half an hour. The solution is made neutral by adding diluted hydrochloric acid, the methanol is distilled off and the oil precipitated from the aqueous mixture is extracted five times with 50 ml of ethyl acetate each. The united ethyl acetate layers are dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated. Thus 39.1 g of 1-(2,4-dimethoxy-benzyl)-4-(hydroxymethyl)-2-azetidinone are obtained. Yield: 96%.

後処理

  1. temperaturecooling
  2. customwithin about half an hour
  3. distillationthe methanol is distilled off
  4. customthe oil precipitated from the aqueous mixture
  5. extractionis extracted five times with 50 ml of ethyl acetate each
  6. dry with materialThe united ethyl acetate layers are dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customthe filtrate is evaporated

出典と根拠

ORDレコード
ord-0929127b37cc44739dd55024c379bfb6
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…