2,4-diamino-5-(7,8-dimethoxy-2-methyl-2H-1-benzopyran-5-ylmethyl)pyrimidine → 2,4-Diamino-5-(7,8-dimethoxy-2-methyl-4H-1-benzopyran-5-ylmethyl)pyrimidine

HRID 280008

반응식

HRID 280008 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][CH:18]([CH3:20])[O:19][C:14]=3[C:13]([O:21][CH3:22])=[C:12]([O:23][CH3:24])[CH:11]=2)=[CH:4][N:3]=1.CC(C)([O-])C.[K+]>CS(C)=O.O>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH2:9][C:10]2[C:15]3[CH2:16][CH:17]=[C:18]([CH3:20])[O:19][C:14]=3[C:13]([O:21][CH3:22])=[C:12]([O:23][CH3:24])[CH:11]=2)=[CH:4][N:3]=1

참가 물질

5

반응물 2

HCID 128497982,4-diamino-5-(7,8-dimethoxy-2-methyl-2H-1-benzopyran-5-ylmethyl)pyrimidineHCID 23665647Potassium tert-butoxide

생성물 1

HCID 128498012,4-Diamino-5-(7,8-dimethoxy-2-methyl-4H-1-benzopyran-5-ylmethyl)pyrimidine수율 85%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

A solution of 2,4-diamino-5-(7,8-dimethoxy-2-methyl-2H-1-benzopyran-5-ylmethyl)pyrimidine (967 mg, 2.94 mmol) and potassium t-butoxide (991 mg, 8.83 mmol) in dimethyl sulfoxide was maintained at 60°-70° for 0.5 hr under nitrogen. The solution was cooled and diluted with water (50 mL). The resulting precipitate (920 mg) was recrystallized from 95% ethanol to give the title compound as white crystals (820 mg, 85%), mp 215°-217° dec., structure confirmed by NMR spectrum. Anal. Calcd for C17H20N4O3 : C, 62.18; H, 6.14; N, 17.06. Found: C, 61.95; H, 6.20; N, 17.00.

후처리

  1. temperatureThe solution was cooled
  2. customThe resulting precipitate (920 mg) was recrystallized from 95% ethanol

출처 및 근거

ORD 기록
ord-49db87b849b242418bfbbfab96edf54d
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587342

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