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Water → HCID 13961960, 화합물

HRID 2309105
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HRID 2309105 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([OH:8])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.O.O1CCOCC1.Cl[CH:19]([F:21])[F:20]>[OH-].[K+].C1OCCOCCOCCOCCOCCOC1>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH:19]([F:21])[F:20])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1
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참가 물질

7

반응물 4

HCID 962WaterHCID 6372ChlorodifluoromethaneHCID 312751,4-DioxaneHCID 178503550HCID 178503550, 화합물

생성물 1

HCID 13961960HCID 13961960, 화합물수율 84.6%

시약·촉매·용매 2

HCID 2855718-Crown-6촉매
HCID 14797
Potassium Hydroxide
용매

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온도
40 °C

실험 절차

6.8 g (0.036 mole) of 4-chloro-6-hydroxy-2-methylthiopyrimidine are suspended in 25 ml 50% potassium hydroxide solution, 25 ml of water and 100 ml of dioxane. After the addition of 0.5 g of 18-crown-6, the reaction mixture is heated to 40° C., and 10 g of chlorodifluoromethane are subsequently introduced over 3 hours. The mixture is then cooled to room temperature, the phases are separated and the organic phase is evaporated to dryness. The residue is crystallised from methanol/water, affording 6.9 g (84.4% of theory) of 4-chloro-6-difluoromethoxy-2-methylthiopyrimidine with a melting point of 36°-37° C. The substance has a boiling point of 76°-78° C. at 0.15 mbar.

후처리

  1. temperatureThe mixture is then cooled to room temperature
  2. customthe phases are separated
  3. customthe organic phase is evaporated to dryness
  4. customThe residue is crystallised from methanol/water

출처 및 근거

ORD 기록
ord-60f65ae7f79d48c8b930d75771cf994d
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04692524

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