Triethylamine → 1-(4-Chlorobenzyloxy)methyl-5-trifluoromethylpyrimidin-2-one

HRID 1719247노트

반응식

HRID 1719247 반응식
C(N(CC)CC)C.[F:8][C:9]([F:18])([F:17])[C:10]1[CH:11]=[N:12][C:13](=[O:16])[NH:14][CH:15]=1.Cl[CH2:20][O:21][CH2:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=1>ClCCl>[Cl:29][C:26]1[CH:27]=[CH:28][C:23]([CH2:22][O:21][CH2:20][N:12]2[CH:11]=[C:10]([C:9]([F:17])([F:8])[F:18])[CH:15]=[N:14][C:13]2=[O:16])=[CH:24][CH:25]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 129465921-Chloro-4-[(chloromethoxy)methyl]benzeneHCID 133170275-(Trifluoromethyl)pyrimidin-2(1H)-one

생성물 1

HCID 133170321-(4-Chlorobenzyloxy)methyl-5-trifluoromethylpyrimidin-2-one수율 91%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
40 °C

실험 절차

Triethylamine (1 mmol) was added to a mixture of 5-trifluoromethyl pyrimidin-2-one (see Preparation 11 of European Patent Publication Ser. No. 0 056 319) (1 mmol) in dichloromethane (10 ml) and the solution stirred for 5 minutes before 4-chlorobenzyl chloromethyl ether (see Preparation 5a and 5b) (1 mmol) in dichloromethane (2 ml) was added. The mixture was stirred at room temperature overnight and at 40° C. for 3 hours before the solvent was distilled off and the residue triturated with water. The product was extracted into chloroform, dried (MgSO4) and evaporated. The residue was washed with ether and dried; yield 91%, m.p. 120° C. 1H NMR (CDCl3): δ4.64 (CH2Ph), 5.38 (NCH2), 7.24 (Ph), 8.11 (H-4, J 3 Hz), 8.74 (H-6, J 3 Hz). IR (KBr): 1680 cm-1 (CO).

후처리

  1. customPreparation 11 of European Patent Publication Ser
  2. additionwas added
  3. distillationwas distilled off
  4. customthe residue triturated with water
  5. extractionThe product was extracted into chloroform
  6. dry with materialdried (MgSO4)
  7. customevaporated
  8. washThe residue was washed with ether
  9. customdried

출처 및 근거

ORD 기록
ord-ed057300f21141de91e5e4b67fea634b
출처 데이터셋
uspto-grants-1985_09
특허 번호
US04539324

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