Sodium Azide → HCID 18594802, 화합물

HRID 2071339노트

반응식

HRID 2071339 반응식
CS(O[CH:6]([CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH2:7][CH2:8][C@@H:9]1[C@@H:13]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:12](=[O:25])[CH2:11][CH2:10]1)(=O)=O.[N-:31]=[N+:32]=[N-:33].[Na+]>CN(C)C=O>[N:31]([CH:6]([CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH2:7][CH2:8][C@@H:9]1[C@@H:13]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:12](=[O:25])[CH2:11][CH2:10]1)=[N+:32]=[N-:33]

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 18594876HCID 18594876, 화합물

생성물 1

HCID 18594802HCID 18594802, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 1.35 g. of ethyl 15-methanesulfonyloxy 9-oxo-prostanoate (Example 90) in 60 ml. of N,N-dimethylformamide containing 1.25 g. of sodium azide is heated on the steam-bath for 18 hours. The cooled solution is poured into 300 ml. of water and the resulting mixture is extracted several times with ether. The combined ether extracts are washed with saturated sodium chloride solution, dried with anhydrous magnesium sulfate and taken to dryness. The residual oil is chromatographed on silica gel to give 737 mg. (62%) of oil; λmax. 4.77 (azido) and 5.78 μ (carbonyl groups).

후처리

  1. additionThe cooled solution is poured into 300 ml
  2. extractionof water and the resulting mixture is extracted several times with ether
  3. washThe combined ether extracts are washed with saturated sodium chloride solution
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe residual oil is chromatographed on silica gel
  6. customto give 737 mg

출처 및 근거

ORD 기록
ord-9a1265adf5e14039a48042be51b6a1d2
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04046787

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