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Bromine → HCID 20071605, 화합물

HRID 981045
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HRID 981045 반응식
[Br:1]Br.[F:3][C:4]([F:23])([F:22])[C:5]1[CH:6]=[CH:7][C:8]([N:11]2[C:16](=[O:17])[CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[N:13]=[CH:12]2)=[N:9][CH:10]=1.O.O.O.C([O-])(=O)C.[Na+]>C(O)(=O)C>[F:23][C:4]([F:3])([F:22])[C:5]1[CH:6]=[CH:7][C:8]([N:11]2[C:16](=[O:17])[CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[N:13]([Br:1])[CH2:12]2)=[N:9][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24408BromineHCID 20071603HCID 20071603, 화합물HCID 23665404Sodium Acetate Trihydrate

생성물 1

HCID 20071605HCID 20071605, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Bromine (0.15 ml) was added in one portion to a suspension of 1-(5-trifluoromethyl-2-pyridyl)-4-trifluoromethylpyrimidin-6-one (compound No. 2 in Table I) (0.5 g) and sodium acetate trihydrate (1.1 g) in acetic acid (4.8 ml). After stirring for 16 hours, the solvent, was removed under reduced pressure, and the residue was poured into water and aqueous sodium bicarbonate solution. Rigourous extraction into diethylether followed by drying over magnesium sulphate and removal of the solvent under reduced pressure, gave 1-(5-trifluoromethyl-2-pyridyl)-3-bromo-4-trifluoromethylpyrimidin-6-one as a pale yellow solid (m.p. 142-143° C.). The compound showed (CDC13) 8.90 (1H,s), 8.80 (1H,s), 8.2 (1H,dg), 8.16 (1H,d).

후처리

  1. customthe solvent, was removed under reduced pressure
  2. additionthe residue was poured into water and aqueous sodium bicarbonate solution
  3. extractionRigourous extraction into diethylether
  4. dry with materialby drying over magnesium sulphate and removal of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-8abd79562d044219bd870115261a5575
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04990512

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