Sodium methanethiolate → 4-Chloro-6-methylthio-2-(phenylmethoxy)pyrimidine

HRID 799

반응식

HRID 799 반응식
[CH3:1][S-:2].[Na+].[Cl:4][C:5]1[CH:10]=[C:9](Cl)[N:8]=[C:7]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:6]=1>C1COCC1>[Cl:4][C:5]1[CH:10]=[C:9]([S:2][CH3:1])[N:8]=[C:7]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:6]=1

참가 물질

4

반응물 2

HCID 4378561Sodium methanethiolateHCID 196938984,6-Dichloro-2-(phenylmethoxy)pyrimidine

생성물 1

HCID 196938764-Chloro-6-methylthio-2-(phenylmethoxy)pyrimidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Aqueous sodium thiomethoxide (15%, 2.75 g, 0.0059×1.0 mol) was added dropwise in 4,6-dichloro-2-(phenylmethoxy)pyrimidine (Compound No. II-26) (1.5 g, 0.0059 mol) dissolved in THF at room temperature. After allowed to react for 2 hours, the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated, then purified on a silica gel column to obtain 4-chloro-6-methylthio-2-(phenylmethoxy)pyrimidine (Compound No. II-15) as an intermediate.

후처리

  1. customto react for 2 hours
  2. customthe reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
  3. washThe organic layer was washed with aqueous saturated sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. custompurified on a silica gel column

출처 및 근거

ORD 기록
ord-bbaa547034cb4578bce2648d1c091a1f
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723412

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