Hydrochloric Acid → HCID 14456866, 화합물

HRID 279780노트

반응식

HRID 279780 반응식
[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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 13505933HCID 13505933, 화합물

생성물 1

HCID 14456866HCID 14456866, 화합물수율 96.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-0929127b37cc44739dd55024c379bfb6
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587049

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