Potassium Carbonate → 2-Amino-6,8-dichloro-9-[1-(2,2-dimethyl-1,3-dioxane4,6-dione-5-yl)eth-2-yl]purine

HRID 846846

반응식

HRID 846846 반응식
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][C:7]([Cl:11])=[N:8]2)=[C:4]([Cl:12])[N:3]=1.[CH3:13][C:14]1([CH3:24])[O:21][C:20](=[O:22])[C:17]2([CH2:19][CH2:18]2)[C:16](=[O:23])[O:15]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[C:7]([Cl:11])[N:8]2[CH2:19][CH2:18][CH:17]2[C:16](=[O:23])[O:15][C:14]([CH3:24])([CH3:13])[O:21][C:20]2=[O:22])=[C:4]([Cl:12])[N:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 797206,6-Dimethyl-5,7-dioxaspiro(2.5)octane-4,8-dioneHCID 54646776,8-Dichloro-9H-purin-2-amine

생성물 1

HCID 198839932-Amino-6,8-dichloro-9-[1-(2,2-dimethyl-1,3-dioxane4,6-dione-5-yl)eth-2-yl]purine수율 58.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2-amino-6,8-dichloropurine (2.04 g), 6,6-dimethyl-5,7-dioxaspiro[2.5]octane-4,8-dione (1.73 g) and anhydrous potassium carbonate (2.12 g) in N,N-dimethylformamide (40 ml) was stirred at room temperature for 18 hours under dry nitrogen. The solvent was evaporated and the residue dissolved in water (60 ml) and acidified from pH 10 to pH 4 with dilute hydrochloric acid. The yellow precipitate was filtered off, washed with water and dried to give 2-amino-6,8-dichloro-9-[1-(2,2-dimethyl-1,3-dioxane4,6-dione-5-yl)eth-2-yl]purine (2.2 g, 50%). T.1.c. r.f. 0.65 (25% methanol-dichloromethane).

후처리

  1. customThe solvent was evaporated
  2. dissolutionthe residue dissolved in water (60 ml)
  3. filtrationThe yellow precipitate was filtered off
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-b1a80c973d1042229fe8a2181048f816
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05138057

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