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Hydrochloric Acid → 6-Amino-2-butoxy-9-[2-(tetrahydro-2H-pyran-4-yl)ethyl]-7,9-dihydro-8H-Purin-8-one

HRID 1011156
ノート
印刷プレビュー

反応式

HRID 1011156 の反応式
[CH2:1]([O:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:23]C)[N:12]2[CH2:15][CH2:16][CH:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)=[C:8]([NH2:25])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl.O.[OH-].[Na+]>CO.O1CCOCC1>[NH2:25][C:8]1[N:7]=[C:6]([O:5][CH2:1][CH2:2][CH2:3][CH3:4])[N:14]=[C:13]2[C:9]=1[NH:10][C:11](=[O:23])[N:12]2[CH2:15][CH2:16][CH:17]1[CH2:18][CH2:19][O:20][CH2:21][CH2:22]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962Water2 回HCID 14798Sodium HydroxideHCID 576997262-Butoxy-8-methoxy-9-[2-(tetrahydro-2H-pyran-4-yl)ethyl]-9H-purin-6-amine

生成物 1

HCID 250251686-Amino-2-butoxy-9-[2-(tetrahydro-2H-pyran-4-yl)ethyl]-7,9-dihydro-8H-Purin-8-one収率 77.7%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
2 回
HCID 312751,4-Dioxane溶媒

実験手順

2-Butoxy-8-methoxy-9-[2-(tetrahydro-2H-pyran-4-yl)ethyl]-9H-purin-6-amine (0.11 g) was dissolved in methanol (2 mL) and treated with 4N hydrogen chloride in 1,4-dioxane (1 mL). The reaction mixture was stirred for 4 hours and was stripped to dryness. Water (2 mL) and methanol (15 mL) were added to the residue and then neutralised by the addition of 2N sodium hydroxide solution. The above was stripped to near dryness (small quantity of water remaining) and the solid thus obtained was filtered (transferred and washed the solid with water (3 mL)). The solid was dried under suction before being dried further in vacuo to afford the title compound as a white solid (82 mg).

後処理

  1. customthe solid thus obtained
  2. filtrationwas filtered (
  3. washwashed the solid with water (3 mL))
  4. customThe solid was dried under suction
  5. custombefore being dried further in vacuo

出典と根拠

ORDレコード
ord-29a35715e40c460b8ea1ad691bfe741c
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977344B2

反応ノート

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