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4,5,6-Trichloro-2-methylpyrimidine → HCID 15003621, 화합물

HRID 2278503
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인쇄 미리보기

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HRID 2278503 반응식
[CH3:1][O-:2].[Na+].[CH3:4][C:5]1[N:10]=[C:9](Cl)[C:8]([Cl:12])=[C:7]([Cl:13])[N:6]=1>C1COCC1>[Cl:13][C:7]1[C:8]([Cl:12])=[C:9]([O:2][CH3:1])[N:10]=[C:5]([CH3:4])[N:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 2310544,5,6-Trichloro-2-methylpyrimidineHCID 10942334Sodium Methoxide

생성물 1

HCID 15003621HCID 15003621, 화합물수율 96.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
5 °C

실험 절차

1.37 g of sodium methoxide are added to a solution of 5 g of 2-methyl-4,5,6-trichloropyrimidine in 41 ml of THF cooled to 5° C. in an ice bath. The ice bath is removed. The suspension is stirred at ambient temperature for 18 hours. The reaction medium is cooled to 5° C. in an ice bath. 20 ml of water and 100 ml of ethyl acetate are added. After settling out, the organic phase is dried over magnesium sulfate, filtered, and concentrated under reduced pressure so as to give 4.73 g of 4,5-dichloro-6-methoxy-2-methylpyrimidine in the form of a colorless oil which crystallizes, the characteristics of which are the following:

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후처리

  1. customThe ice bath is removed
  2. temperatureThe reaction medium is cooled to 5° C. in an ice bath
  3. addition20 ml of water and 100 ml of ethyl acetate are added
  4. dry with materialthe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure so as

출처 및 근거

ORD 기록
ord-9879af4a3e9f413faeb4d7b3182b496b
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09133168B2

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