Ammonium Hydroxide → 9-Butyl-8-(2,5-Dimethoxy-Benzyl)-9h-Purin-6-Ylamine

HRID 1295468노트

반응식

HRID 1295468 반응식
Cl[C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([CH2:15][C:16]1[CH:21]=[C:20]([O:22][CH3:23])[CH:19]=[CH:18][C:17]=1[O:24][CH3:25])[N:6]2[CH2:11][CH2:12][CH2:13][CH3:14].[NH4+:26].[OH-]>O1CCOCC1>[CH3:25][O:24][C:17]1[CH:18]=[CH:19][C:20]([O:22][CH3:23])=[CH:21][C:16]=1[CH2:15][C:5]1[N:6]([CH2:11][CH2:12][CH2:13][CH3:14])[C:7]2[C:3]([N:4]=1)=[C:2]([NH2:26])[N:10]=[CH:9][N:8]=2

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 858276576-chloro-8-(2,5-dimethoxybenzyl)-N9-butyl purine

생성물 1

HCID 4489699-Butyl-8-(2,5-Dimethoxy-Benzyl)-9h-Purin-6-Ylamine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of 6-chloro-8-(2,5-dimethoxybenzyl)-N9-butyl purine (1 mmol) in dioxane was added 28% NH4OH (50 mmol) and the mixture was then heated at 100 C in a seal tube for 48 h. Solvent was removed by azeotrope distillation with toluene. Purification on a silica gel column (see above) gave pure 8-(2,5-dimethoxybenzyl)-9-butyl adenine, 1.1. Rf=0.35 in 5% MeOH in EtOHAc. 1H NMR (DMSO-d6) δ 8.08 (s, 1H), 7.04 (br s, 2H), 6.94 (d, 1H), 6.80 (dd, 1H), 6.66 (d, 1H), 4.14 (s, 2H), 4.04 (t, 2H), 3.72 (s, 3H), 3.63 (s, 3H), 1.52 (m, 2H), 1.22 (m, 2H), 0.82 (t, 3H).

후처리

  1. temperaturethe mixture was then heated at 100 C in a seal tube for 48 h
  2. customSolvent was removed by azeotrope distillation with toluene
  3. customPurification on a silica gel column (see above)

출처 및 근거

ORD 기록
ord-51eca18288364916976b90311ead8a22
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07241890B2

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