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Bromine → HCID 178478024、化合物

HRID 1376318
ノート
印刷プレビュー

反応式

HRID 1376318 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:12]=[CH:11][NH:10][N:9]=1.[Br:13]Br>C(O)(=O)C.C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:12]([Br:13])=[CH:11][NH:10][N:9]=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 2

HCID 24408Bromine2 回HCID 178478013HCID 178478013、化合物

生成物 1

HCID 178478024HCID 178478024、化合物収率 65.3%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒3 回HCID 6344Dichloromethane溶媒

実験手順

3.5 g of 3-(2-chlorophenyl)-1H-pyrazole, prepared as in Example 9, are dissolved, at room temperature and with stirring, in 20 ml of acetic acid. A solution of 3.76 g (0.0235 mol) of bromine in 20 ml of acetic acid is then run dropwise into the reaction mixture. Stirring is maintained for 1 hour at room temperature and then the acetic acid and the excess bromine are driven off under reduced pressure. The residue is taken up in methylene chloride and this organic solution is washed with an aqueous bicarbonate solution, then with water and then dried over MgSO4 before being concentrated to dryness. The residue is recrystallised from pentane. 3.3 g (0.0128 mol) of 3-(2'-chlorophenyl)-4-bromo-1H-pyrazole are obtained, which melts at 80° C. (yield 65%) (compound 94)

後処理

  1. dissolutionare dissolved, at room temperature
  2. washthis organic solution is washed with an aqueous bicarbonate solution
  3. dry with materialwith water and then dried over MgSO4
  4. concentrationbefore being concentrated to dryness
  5. customThe residue is recrystallised from pentane

出典と根拠

ORDレコード
ord-fe0049d11d4d420383f6d5c78f918728
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05663119

反応ノート

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