HCID 86734335, 화합물 → cis-3-Amino-4-oxo-2-p-toluenesulfonyloxymethylazetidine

HRID 2050391노트

반응식

HRID 2050391 반응식
[N:1]([C@H:4]1[C:7](=[O:8])[NH:6][C@H:5]1[CH2:9][O:10][S:11]([C:14]1[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=1)(=[O:13])=[O:12])=[N+]=[N-]>C(O)(=O)C.[Zn]>[NH2:1][C@H:4]1[C:7](=[O:8])[NH:6][C@H:5]1[CH2:9][O:10][S:11]([C:14]1[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=1)(=[O:13])=[O:12]

참가 물질

4

반응물 1

HCID 86734335HCID 86734335, 화합물

생성물 1

HCID 86734334cis-3-Amino-4-oxo-2-p-toluenesulfonyloxymethylazetidine

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

실험 절차

Zinc dust (2.0 g, 0.03 mole) was slowly added with cooling to a solution of 5.0 g (0.011 mole) of cis-3-azido-4-oxo-2-p-toluenesulfonyloxymethylazetidine in 50 ml of 50% aqueous acetic acid. The reaction mixture was stirred for 30 minutes and filtered. The solids were washed with water and the filtrate was saturated with hydrogen sulfide, filtered and concentrated to near dryness. The residue was dissolved in ethyl acetate-water and the pH was adjusted to 8.0 by addition of sodium carbonate and sodium hydroxide solutions. The layers were separated and the aqueous phase was extracted twice with ethyl acetate. The extracts were combined, dried (MgSO4) and evaporated to dryness to give the title compound.

후처리

  1. filtrationfiltered
  2. washThe solids were washed with water
  3. filtrationfiltered
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in ethyl acetate-water
  6. additionthe pH was adjusted to 8.0 by addition of sodium carbonate and sodium hydroxide solutions
  7. customThe layers were separated
  8. extractionthe aqueous phase was extracted twice with ethyl acetate
  9. dry with materialdried (MgSO4)
  10. customevaporated to dryness

출처 및 근거

ORD 기록
ord-b8be26f351c148ee940dadbe0827ce8b
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04200572

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