Water → Phenyl 5-methylisoxazol-3-ylcarbamate

HRID 853279ノート

反応式

HRID 853279 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 4519264Phenyl 5-methylisoxazol-3-ylcarbamate収率 68%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-aad17c9c199745dfa6517d4acb744da7
出典データセット
uspto-grants-2007_08
特許番号
US07253286B2

反応ノート

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