Sodium Azide → HCID 53771027, 화합물

HRID 621083노트

반응식

HRID 621083 반응식
C(O[C@@H:5]1[NH:8][C:7](=[O:9])[C@H:6]1[NH:10][C:11]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)(=O)C.[N-:30]=[N+:31]=[N-:32].[Na+]>CO.O>[N:30]([C@H:5]1[NH:8][C:7](=[O:9])[C@H:6]1[NH:10][C:11]([C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[N+:31]=[N-:32]

참가 물질

5

반응물 2

HCID 33557Sodium AzideHCID 53918863HCID 53918863, 화합물

생성물 1

HCID 53771027HCID 53771027, 화합물수율 35.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 3.0 g of (3S,4S)-4-acetoxy-3-tritylamino-2-oxoazetidine in 50 ml of methanol is added a solution of 0.65 g of sodium azide in 5 ml of water under ice-cooling, followed by stirring for two hours at 40°-50° C. The solvent is distilled off under reduced pressure. To the residue is added ethyl acetate, and the organic layer is separated, which is washed with water and concentrated. The residue is purified on a silica-gel column (ethyl acetate:n-hexane=1:1) to give 1.01 g of (3S,4R)-4-azido-3-tritylamino-2-oxoazetidine.

후처리

  1. temperaturecooling
  2. distillationThe solvent is distilled off under reduced pressure
  3. additionTo the residue is added ethyl acetate
  4. customthe organic layer is separated
  5. washwhich is washed with water
  6. concentrationconcentrated
  7. customThe residue is purified on a silica-gel column (ethyl acetate:n-hexane=1:1)

출처 및 근거

ORD 기록
ord-7baed78ab9c34cc9bb02b01490b350e7
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04822788

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