Hydrochloric Acid → 6-Amino-2-(butylamino)-9-[(2,2-dimethyltetrahydro-2H-pyran-4-yl)methyl]-7,9-dihydro-8H-purin-8-one

HRID 1011173ノート

反応式

HRID 1011173 の反応式
[CH2:1]([NH:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:24]C)[N:12]2[CH2:15][CH:16]2[CH2:21][CH2:20][O:19][C:18]([CH3:23])([CH3:22])[CH2:17]2)=[C:8]([NH2:26])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl>CO.O1CCOCC1>[NH2:26][C:8]1[N:7]=[C:6]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])[N:14]=[C:13]2[C:9]=1[NH:10][C:11](=[O:24])[N:12]2[CH2:15][CH:16]1[CH2:21][CH2:20][O:19][C:18]([CH3:23])([CH3:22])[CH2:17]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 57699692N2-Butyl-9-[(2,2-dimethyltetrahydro-2H-pyran-4-yl)methyl]-8-methoxy-9H-purine-2,6-diamine

生成物 1

HCID 576997186-Amino-2-(butylamino)-9-[(2,2-dimethyltetrahydro-2H-pyran-4-yl)methyl]-7,9-dihydro-8H-purin-8-one収率 52.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of N2-butyl-9-[(2,2-dimethyltetrahydro-2H-pyran-4-yl)methyl]-8-methoxy-9H-purine-2,6-diamine (73 mg) in MeOH (2 mL) was treated with 4N HCl in 1,4-dioxane (1 mL) and was stirred for 4 h. The reaction was evaporated and the residue treated with water then basified with saturated sodium bicarbonate solution. The resulting solid was filtered, washed with water and dried. The solid was re-precipitated from ether/light petrol to give the title compound (37 mg).

後処理

  1. customThe reaction was evaporated
  2. additionthe residue treated with water
  3. filtrationThe resulting solid was filtered
  4. washwashed with water
  5. customdried
  6. customThe solid was re-precipitated from ether/light petrol

出典と根拠

ORDレコード
ord-d6f777a6bab7490680745212478bb275
出典データセット
uspto-grants-2011_07
特許番号
US07977344B2

反応ノート

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