Sodium Azide → 3-Azido-1-benzhydrylazetidine

HRID 323604

반응식

HRID 323604 반응식
[CH:1]([N:14]1[CH2:17][CH:16](OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:15]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N-:29]=[N+:30]=[N-:31].[Na+]>CN(C=O)C>[N:29]([CH:16]1[CH2:17][N:14]([CH:1]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:15]1)=[N+:30]=[N-:31]

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 155126511-Benzhydrylazetidin-3-yl 4-methylbenzenesulfonate

생성물 1

HCID 155126523-Azido-1-benzhydrylazetidine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 9 (11.5 g, 31.8 mmol) and sodium azide (4.12 g, 64 mmol) in 250 ml of DMF was heated to 70° C. for 24 hours. After cooling to room temperature the solvent was removed in vacuo and the residue partitioned between chloroform and water. The organics were dried over MgSO4, filtered and the solvent removed in vacuo. The crude product was purified by chromatography on silica gel (8:1 hexane: ethyl acetate) afforded the title compound.

후처리

  1. customwas removed in vacuo
  2. customthe residue partitioned between chloroform and water
  3. dry with materialThe organics were dried over MgSO4
  4. filtrationfiltered
  5. customthe solvent removed in vacuo
  6. customThe crude product was purified by chromatography on silica gel (8:1 hexane: ethyl acetate)

출처 및 근거

ORD 기록
ord-b1217393730944209c1603dc36d443ea
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06214832B1

연결된 노트

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