Maleic Anhydride → 2,4-Diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine Maleate

HRID 280003

반응식

HRID 280003 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH2:9][C:10]2[C:15]3[CH:16]=[CH:17][CH2:18][O:19][C:14]=3[C:13]([O:20][CH3:21])=[C:12]([O:22][CH3:23])[CH:11]=2)=[CH:4][N:3]=1.[C:24]([OH:31])(=[O:30])/[CH:25]=[CH:26]\[C:27]([OH:29])=[O:28].C1(=O)OC(=O)C=C1>O>[C:24]([OH:31])(=[O:30])/[CH:25]=[CH:26]\[C:27]([OH:29])=[O:28].[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH2:9][C:10]2[C:15]3[CH:16]=[CH:17][CH2:18][O:19][C:14]=3[C:13]([O:20][CH3:21])=[C:12]([O:22][CH3:23])[CH:11]=2)=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 7923Maleic AnhydrideHCID 444266Maleic AcidHCID 128497722,4-diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine

생성물 1

HCID 704045882,4-Diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine Maleate수율 94.9%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
0 °C

실험 절차

To 2,4-diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine (3.90 g, 12.4 mmol) in 200 mL of boiling water was added a solution of maleic acid, prepared by dissolution of maleic anhydride (1.25 g, 12.7 mmol) in 50 mL of hot water. After cooling to 0° C., the crystalline salt was filtered, washed with cold water, and dried at 75° C. to give 5.07 g (94.9%) of the title compound. Anal. Calcd for C20H22N4O7 : C, 55.81; H, 5.15; N, 13.02. Found: C, 55.78; H, 5.18; N, 12.98.

후처리

  1. filtrationthe crystalline salt was filtered
  2. washwashed with cold water
  3. customdried at 75° C.

출처 및 근거

ORD 기록
ord-c0805707126b40219d6ea6e6a046917c
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587342

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