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

반응식

HRID 131561 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aa2686d9fed644a8b4ea57c0b60b8015
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07384950B2

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