Hydroxylamine → 2-Acetyl-4-(pyrid-2-yl)-pyrimidine oxime

HRID 933

반응식

HRID 933 반응식
[C:1]([C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=2)[CH:7]=[CH:6][N:5]=1)(=O)[CH3:2].[NH2:16][OH:17].C([O-])(=O)C.[Na+]>C(O)C.O>[C:1](=[N:16][OH:17])([C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=2)[CH:7]=[CH:6][N:5]=1)[CH3:2]

참가 물질

6

반응물 3

HCID 787HydroxylamineHCID 517045Sodium AcetateHCID 196942132-Acetyl-4-(pyrid-2-yl)-pyrimidine

생성물 1

HCID 1363959922-Acetyl-4-(pyrid-2-yl)-pyrimidine oxime수율 91.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

A solution of 2-acetyl-4-(pyrid-2-yl)-pyrimidine (1.0 g), hydroxylamine (0.39 g) and sodium acetate (0.62 g) in a mixture of ethanol (10 ml) and water (2 ml) was heated to reflux for 1.5 hours. The reaction was then poured into water the precipitate filtered and washed with hexane to give 2-acetyl-4-(pyrid-2-yl)-pyrimidine oxime (0.98 g, 91% yield) as a white crystalline solid m.p. 196°-8° C.; 1H NMR: 2.50(3H,s); 7.42(1H,m); 7.88(1H,m); 8.30(1H,d); 8.59(1H,d); 8.74(1H,d); 8.90(1H,d); 10.85(1H,brs) ppm.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 1.5 hours
  3. filtrationfiltered
  4. washwashed with hexane

출처 및 근거

ORD 기록
ord-25314cafe14044c4a971af24b93211f4
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723473

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