Water → Phenyl 5-methylisoxazol-3-ylcarbamate

HRID 853279노트

반응식

HRID 853279 반응식
[NH2:1][C:2]1[CH:6]=[C:5]([CH3:7])[O:4][N:3]=1.[C:8](Cl)(=[O:16])[O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.O>O1CCCC1.N1C=CC=CC=1>[CH3:7][C:5]1[O:4][N:3]=[C:2]([NH:1][C:8](=[O:16])[O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:6]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 15891Phenyl chloroformateHCID 661723-Amino-5-methylisoxazole

생성물 1

HCID 4519264Phenyl 5-methylisoxazol-3-ylcarbamate수율 68%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8028Tetrahydrofuran용매

실험 절차

3-Amino-5-methylisoxazole (1.00 g) purchased from Aldrich Co. was dissolved in tetrahydrofuran (20 ml) and pyridine (1.5 ml), and after cooling to 0° C. under a nitrogen atmosphere, phenyl chlorocarbonate (1.4 ml) was added and the mixture was stirred at room temperature for 2 hours. Water was added, extraction was performed twice with ethyl acetate, and then the organic layers were combined, washed with water and saturated brine in that order, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The obtained residue was triturated with diethyl ether and n-hexane to obtain the title compound (1.54 g) (68% yield).

후처리

  1. extractionextraction
  2. washwashed with water and saturated brine in that order
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe obtained residue was triturated with diethyl ether and n-hexane

출처 및 근거

ORD 기록
ord-aad17c9c199745dfa6517d4acb744da7
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253286B2

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