6-Chloro-3-methyl-1-propyl-2,4(1H,3H)-pyrimidinedione → 6-Mercapto-3-methyl-1-propyl-pyrimidine-2,4(1H,3H)-dione

HRID 131561

反応式

HRID 131561 の反応式
Cl[C:2]1[N:7]([CH2:8][CH2:9][CH3:10])[C:6](=[O:11])[N:5]([CH3:12])[C:4](=[O:13])[CH:3]=1.O.[SH-:15].[Na+]>C(O)C>[SH:15][C:2]1[N:7]([CH2:8][CH2:9][CH3:10])[C:6](=[O:11])[N:5]([CH3:12])[C:4](=[O:13])[CH:3]=1

参加物

4

反応物 2

HCID 8169336-Chloro-3-methyl-1-propyl-2,4(1H,3H)-pyrimidinedioneHCID 16211346Sodium hydrosulfide hydrate

生成物 1

HCID 866227106-Mercapto-3-methyl-1-propyl-pyrimidine-2,4(1H,3H)-dione

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 6-chloro-3-methyl-1-propyl-pyrimidine-2,4(1H,3H)-dione (3.76 g), sodium hydrosulphide hydrate (6 g) and ethanol (100 ml) was stirred at room temperature for 48 hours then concentrated in vacuo. The residue was dissolved in water (500 ml) and washed with ethyl acetate (2×100 ml). The aqueous phase was acidified with dilute hydrochloric acid, then extracted with ethyl acetate (3×100 ml). The combined organic phase was dried (MgSO4) and evaporated to leave a pale yellow solid which was used directly in the next step.

後処理

  1. concentrationthen concentrated in vacuo
  2. dissolutionThe residue was dissolved in water (500 ml)
  3. washwashed with ethyl acetate (2×100 ml)
  4. extractionextracted with ethyl acetate (3×100 ml)
  5. dry with materialThe combined organic phase was dried (MgSO4)
  6. customevaporated
  7. customto leave a pale yellow solid which

出典と根拠

ORDレコード
ord-aa2686d9fed644a8b4ea57c0b60b8015
出典データセット
uspto-grants-2008_06
特許番号
US07384950B2

関連ノート

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