Hydrochloric Acid → 6-Amino-2-[(tetrahydro-2-furanylmethyl)oxy]-9-(tetrahydro-2H-pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-one

HRID 1011190ノート

反応式

HRID 1011190 の反応式
C[O:2][C:3]1[N:4]([CH2:20][CH:21]2[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[C:5]2[C:10]([N:11]=1)=[C:9]([NH2:12])[N:8]=[C:7]([O:13][CH2:14][CH:15]1[CH2:19][CH2:18][CH2:17][O:16]1)[N:6]=2.Cl.[OH-].[Na+]>CO.O1CCOCC1>[NH2:12][C:9]1[N:8]=[C:7]([O:13][CH2:14][CH:15]2[CH2:19][CH2:18][CH2:17][O:16]2)[N:6]=[C:5]2[C:10]=1[NH:11][C:3](=[O:2])[N:4]2[CH2:20][CH:21]1[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 576996338-(Methoxy)-2-[(tetrahydro-2-furanylmethyl)oxy]-9-(tetrahydro-2H-Pyran-4-ylmethyl)-9H-purin-6-amine

生成物 1

HCID 576997746-Amino-2-[(tetrahydro-2-furanylmethyl)oxy]-9-(tetrahydro-2H-pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-one収率 78.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

8-(Methoxy)-2-[(tetrahydro-2-furanyl methyl)oxy]-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purin-6-amine (0.1500 g) was dissolved in methanol (10 mL). To this solution was added 4N hydrogen chloride in 1,4-dioxane (2 mL). The reaction mixture was stirred for 5 hours at room temperature. The reaction mixture was evaporated under reduced pressure and then water (3 mL) and methanol (3 mL) was added to the residue to give a finely divided suspension. This was neutralised (to pH 7) by the addition of 2N sodium hydroxide and then evaporated under reduced pressure to dryness. Water (3 mL) was then added to the residue and the resultant white suspension of solid was isolated by filtration under suction. The solid was washed with methanol (1 mL) and then air-dried under suction. The solid was then dried further to constant weight under vacuo at 50° C. (˜1 hour). This gave the title compound as a white solid (0.1130 g)

後処理

  1. customThe reaction mixture was evaporated under reduced pressure
  2. additionwater (3 mL) and methanol (3 mL) was added to the residue
  3. customto give a finely divided suspension
  4. customevaporated under reduced pressure to dryness
  5. additionWater (3 mL) was then added to the residue
  6. additionthe resultant white suspension of solid
  7. customwas isolated by filtration under suction
  8. washThe solid was washed with methanol (1 mL)
  9. customair-dried under suction
  10. customThe solid was then dried further to constant weight under vacuo at 50° C. (˜1 hour)

出典と根拠

ORDレコード
ord-b9f300880d38435798995279a2b01dfa
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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