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Hydrochloric Acid → HCID 21258162、化合物

HRID 635207
ノート
印刷プレビュー

反応式

HRID 635207 の反応式
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][CH2:19][CH3:20])[C:13](=[O:21])[N:12]([CH2:22][CH2:23][C:24]([O:26]C)=[O:25])[C:11]=2[N:10]=[C:9]1[C:28]([CH3:31])([CH3:30])[CH3:29])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O1CCCC1.[Li+].[OH-].Cl>O>[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][CH2:19][CH3:20])[C:13](=[O:21])[N:12]([CH2:22][CH2:23][C:24]([OH:26])=[O:25])[C:11]=2[N:10]=[C:9]1[C:28]([CH3:29])([CH3:31])[CH3:30])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 21258170HCID 21258170、化合物

生成物 1

HCID 21258162HCID 21258162、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
5 °C

実験手順

4.6 g (10.8 mmol) of 7-benzyl-8-(tert.-butyl)-3-(2-methoxycarbonylethyl)-1-n-propyl-xanthine are dissolved 50 ml of tetrahydrofuran and 120 ml of water and 3.24 g of LiOH×H2O are added successively with stirring. After about 16 hours' stirring at ambient temperature, the mixture is cooled to about 5° C. and adjusted to pH 5 with 2N HCl (aq.). The organic solvent is largely distilled off in vacuo and the aqueous phase remaining is extracted twice with 150 ml of dichloromethane. The organic phase is dried over MgSO4 and the solvent is distilled off in vacuo. The crude product remaining is purified by chromatography on silica gel (dichloromethane:methanol 90:10). Yield: 3.1 g (88%), amorphous solid.

後処理

  1. additionare added successively
  2. stirringAfter about 16 hours' stirring at ambient temperature
  3. distillationThe organic solvent is largely distilled off in vacuo
  4. extractionthe aqueous phase remaining is extracted twice with 150 ml of dichloromethane
  5. dry with materialThe organic phase is dried over MgSO4
  6. distillationthe solvent is distilled off in vacuo
  7. customThe crude product remaining is purified by chromatography on silica gel (dichloromethane:methanol 90:10)

出典と根拠

ORDレコード
ord-220995ad001d491aaf6c9c599d67e47d
出典データセット
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06187780B1

反応ノート

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