Fumaric Acid → AZD-8055 fumarate

HRID 218357노트

반응식

HRID 218357 반응식
[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[N:9]=[C:10]([N:28]2[CH2:33][CH2:32][O:31][CH2:30][C@@H:29]2[CH3:34])[C:11]2[CH:17]=[CH:16][C:15]([C:18]3[CH:19]=[CH:20][C:21]([O:26][CH3:27])=[C:22]([CH2:24][OH:25])[CH:23]=3)=[N:14][C:12]=2[N:13]=1.[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]/[C:38]([OH:40])=[O:39]>O>[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]/[C:38]([OH:40])=[O:39].[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[N:9]=[C:10]([N:28]2[CH2:33][CH2:32][O:31][CH2:30][C@@H:29]2[CH3:34])[C:11]2[CH:17]=[CH:16][C:15]([C:18]3[CH:19]=[CH:20][C:21]([O:26][CH3:27])=[C:22]([CH2:24][OH:25])[CH:23]=3)=[N:14][C:12]=2[N:13]=1

참가 물질

4

반응물 2

HCID 444972Fumaric AcidHCID 25262965Azd8055

생성물 1

HCID 44537932AZD-8055 fumarate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
92 °C

실험 절차

(5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol (10.00 g (96% w/w, 20.6 moles), fumaric Acid (2.63 g, 22.7 mmoles), water (84 ml) and methylated spirit industrial 74 O.P. (16.0 ml) were charged to a 250 ml reactor and heated to reflux (92° C.). The hot solution was filtered to remove extraneous matter. The filter was washed with a mixture of water (17 ml and methylated spirit industrial 74 O.P. (3 ml). On cooling the combined filtrates product precipitated. Product was isolated, washed with methylated spirit industrial 74 O.P. and dried to yield 10.12 g of (5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol Fumarate as a yellow solid.

후처리

  1. addition(16.0 ml) were charged to a 250 ml reactor
  2. temperatureheated
  3. filtrationThe hot solution was filtered
  4. customto remove extraneous matter
  5. washThe filter was washed with a mixture of water (17 ml and methylated spirit industrial 74 O.P
  6. temperatureOn cooling the combined filtrates product
  7. customprecipitated
  8. customProduct was isolated
  9. washwashed with methylated spirit industrial 74 O.P
  10. customand dried

출처 및 근거

ORD 기록
ord-8cc3de73fb3845a8ac8267a46faf47d1
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198441B2

반응 노트

불러오는 중…