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

反応式

HRID 846846 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b1a80c973d1042229fe8a2181048f816
出典データセット
uspto-grants-1992_08
特許番号
US05138057

関連ノート

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