Methanol → 1-(2-Isopropylamino-6-methyl-pyrimidin-4-yl)-ethanone oxime

HRID 2069469노트

반응식

HRID 2069469 반응식
Cl.[NH2:2][OH:3].[CH:4]([NH:7][C:8]1[N:13]=[C:12]([C:14](=O)[CH3:15])[CH:11]=[C:10]([CH3:17])[N:9]=1)([CH3:6])[CH3:5].CO>O.[OH-].[Na+]>[CH:4]([NH:7][C:8]1[N:13]=[C:12]([C:14](=[N:2][OH:3])[CH3:15])[CH:11]=[C:10]([CH3:17])[N:9]=1)([CH3:6])[CH3:5]

참가 물질

6

반응물 3

HCID 887MethanolHCID 443297Hydroxyamine hydrochlorideHCID 685106621-(2-Isopropylamino-6-methyl-pyrimidin-4-yl)-ethanone

생성물 1

HCID 1363463701-(2-Isopropylamino-6-methyl-pyrimidin-4-yl)-ethanone oxime수율 83.6%

시약·촉매·용매 2

HCID 962Water용매HCID 14798Sodium Hydroxide용매

반응 조건

온도
80 °C

실험 절차

A solution of hydroxylamine hydrochloride (737 mg, 10.6 mmol) in water (3.0 mL) and 1 N aq. NaOH (11 mL) is added to 1-(2-isopropylamino-6-methyl-pyrimidin-4-yl)-ethanone (1.71 g, 8.85 mmol). The solution is stirred at 80° C. for 2 h and MeOH is added to maintain homogeneity of the mixture. The mixture is cooled to rt and the precipitate that forms is collected, washed with water and dried in vacuo to give 1-(2-isopropylamino-6-methyl-pyrimidin-4-yl)-ethanone oxime (1.54 g) as a yellow solid; LC-MS: tR=0.72 min, [M+H]+=209.52; 1H NMR (D6-DMSO): δ 1.15 (d, J=6.5 Hz, 6H), 2.10 (s, 3H), 2.25 (s, 3H), 4.07 (m, 1H), 6.80 (s, 1H), 6.86 (d, J=7.5 Hz, 1H), 11.62 (s, 1H).

후처리

  1. temperatureto maintain homogeneity of the mixture
  2. temperatureThe mixture is cooled to rt
  3. customthe precipitate that forms is collected
  4. washwashed with water
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-5c6b09d1722447c68c9eef1b3a1a2883
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299086B2

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