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

HRID 900741

반응식

HRID 900741 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 (6.0 g) and ethanol (100 ml) was stirred at room temperature for 48 h then concentrated under reduced pressure. 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 concentrated in vacuo to give a pale yellow solid which was used directly in the next step.

후처리

  1. concentrationthen concentrated under reduced pressure
  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. concentrationconcentrated in vacuo
  7. customto give a pale yellow solid which

출처 및 근거

ORD 기록
ord-568deac23f4248b48d9e5e90da645807
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07361660B2

연결된 노트

불러오는 중…