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Ethanol → HCID 20195958, 화합물

HRID 653184
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HRID 653184 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([CH2:9][C:10]2[CH:11]=[N:12][C:13]([CH3:16])=[CH:14][CH:15]=2)=[CH:4][N:3]=1.[Na].[CH2:18]([OH:20])[CH3:19]>>[Cl:1][C:2]1[N:7]=[C:6]([O:20][CH2:18][CH3:19])[C:5]([CH2:9][C:10]2[CH:11]=[N:12][C:13]([CH3:16])=[CH:14][CH:15]=2)=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 702Ethanol2회HCID 5360545SodiumHCID 133743332,4-Dichloro-5-[(6-methyl-3-pyridinyl)methyl]pyrimidine

생성물 1

HCID 20195958HCID 20195958, 화합물수율 90%

실험 절차

To a stirred solution of 8.1 g (32 mmol) of 2,4-dichloro-5-[(6-methyl-3-pyridinyl)methyl]pyrimidine prepared as in Example 1 in 200 ml of ethanol at 10° was added dropwise over 1 hour a solution of 0.8 g (35 mg-atom) of sodium metal in 100 ml of ethanol. The resulting mixture was stirred for 18 hours at room temperature, concentrated, and the resulting oil dissolved in 100 ml of ethyl acetate. The resulting solution was washed with water, dried over sodium sulfate, filtered and concentrated to give 7.6 g (0.0288 mmol, 90%) of 2-chloro-4-ethoxy-5-[(6-methyl-3-pyridinyl)methyl]pyrimidine; MS(FD)m/e 263 parent ion.

후처리

  1. concentrationconcentrated
  2. dissolutionthe resulting oil dissolved in 100 ml of ethyl acetate
  3. washThe resulting solution was washed with water
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d75b5b90b7a94baa8d5e1679e4e49f58
출처 데이터셋
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04675406

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