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Dimethylformamide → HCID 178503553, 화합물

HRID 2353639
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HRID 2353639 반응식
Cl[CH2:2][C:3]1[N:8]=[C:7]([S:9][CH3:10])[N:6]=[C:5]([OH:11])[CH:4]=1.[Na+].[CH3:13][S:14]([O-:16])=[O:15].CN(C=O)C>C(#N)C>[CH3:10][S:9][C:7]1[N:6]=[C:5]([OH:11])[CH:4]=[C:3]([CH2:2][S:14]([CH3:13])(=[O:16])=[O:15])[N:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 2733271Sodium methanesulfinateHCID 178503549HCID 178503549, 화합물

생성물 1

HCID 178503553HCID 178503553, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
100 °C

실험 절차

6-(Chloromethyl)-2-methylsulfanyl-pyrimidin-4-ol (19.07 g, 100 mmol) was suspended in acetonitrile (400 ml). To this stirring suspension was added methanesulphinic acid sodium salt (12.255 g, 120 mmol) and DMF (100 ml). The reaction was then heated to 100° C. to give a dark suspension and monitored by LCMS. Once complete, the solvents were removed and the resultant product added to 1:1 MeOH:DCM (200 ml) and acidified with acetic acid (10 ml). The resultant precipitate was collected, washed with water (200 ml) and MeOH (100 ml) and dried overnight in vacuo to afford the title compound as a white solid, 16.45 g.

후처리

  1. customto give a dark suspension
  2. customOnce complete, the solvents were removed
  3. additionthe resultant product added to 1:1 MeOH
  4. customThe resultant precipitate was collected
  5. washwashed with water (200 ml) and MeOH (100 ml)
  6. customdried overnight in vacuo

출처 및 근거

ORD 기록
ord-f7a7b94b7bf14e9884ad6504c755d549
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07750003B2

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