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Bromine → HCID 20071605、化合物

HRID 981045
ノート
印刷プレビュー

反応式

HRID 981045 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24408BromineHCID 20071603HCID 20071603、化合物HCID 23665404Sodium Acetate Trihydrate

生成物 1

HCID 20071605HCID 20071605、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8abd79562d044219bd870115261a5575
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04990512

反応ノート

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