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Hydrochloric Acid → N-({6-[(2,2-Diphenylethyl)amino]-9H-purin-2-yl}methyl)-N'-[2-(1-piperidinyl)ethyl]urea

HRID 1293022
ノート
印刷プレビュー

反応式

HRID 1293022 の反応式
[C:1]1([CH:7]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[CH2:8][NH:9][C:10]2[N:18]=[C:17]([CH2:19][NH:20][C:21]([NH:23][CH2:24][CH2:25][N:26]3[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]3)=[O:22])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][N:14]3C2CCCCO2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl>CO>[C:38]1([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:8][NH:9][C:10]2[N:18]=[C:17]([CH2:19][NH:20][C:21]([NH:23][CH2:24][CH2:25][N:26]3[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]3)=[O:22])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][NH:14]3)[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21360613N-({6-[(2,2-Diphenylethyl)amino]-9-tetrahydro-2H-pyran-2-yl-9H-purin-2-yl}methyl)-N'-[2-(1-piperidinyl)ethyl]urea

生成物 1

HCID 178523406N-({6-[(2,2-Diphenylethyl)amino]-9H-purin-2-yl}methyl)-N'-[2-(1-piperidinyl)ethyl]urea収率 100.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of N-({6-[(2,2-diphenylethyl)amino]-9-tetrahydro-2H-pyran-2-yl-9H-purin-2-yl}methyl)-N′-[2-(1-piperidinyl)ethyl]urea (300 mg, 0.51 mmol) (Preparation 4) in methanol (150 ml) was treated with aqueous hydrochloric acid (2M, 100 ml). The reaction mixture was stirred at room temperature for 2 hours. The solvent volume was then reduced to 100 ml by evaporation under reduced pressure. Saturated aqueous sodium hydrogen carbonate solution (50 ml) and ethyl acetate (200 ml) were added. The two phases were separated. The organic layer was washed with saturated aqueous sodium chloride solution (100 ml), dried (anhydrous magnesium sulphate) and evaporated to give the title compound as a solid (255 mg).

後処理

  1. customThe solvent volume was then reduced to 100 ml by evaporation under reduced pressure
  2. additionSaturated aqueous sodium hydrogen carbonate solution (50 ml) and ethyl acetate (200 ml) were added
  3. customThe two phases were separated
  4. washThe organic layer was washed with saturated aqueous sodium chloride solution (100 ml)
  5. dry with materialdried (anhydrous magnesium sulphate)
  6. customevaporated

出典と根拠

ORDレコード
ord-57940ed529ce42a09b37e338e950aa51
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07238676B2

反応ノート

読み込み中…

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