Allyl bromide → HCID 20507740、化合物

HRID 128079ノート

反応式

HRID 128079 の反応式
[N:1]1([C:7]2[N:8]=[C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=[C:10]3[N:11]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].[CH2:23](Br)[CH:24]=[CH2:25]>CS(C)=O.[Cl-].[Na+].O>[CH2:25]([N:4]1[CH2:5][CH2:6][N:1]([C:7]2[N:11]=[C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=[C:9]3[N:8]=2)[CH2:2][CH2:3]1)[CH:24]=[CH2:23]

参加物

6

反応物 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 13036368HCID 13036368、化合物

生成物 1

HCID 20507740HCID 20507740、化合物収率 72.6%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒2 回HCID 57417360Sodium chloride; water溶媒

実験手順

A mixture of 2-(1-piperazinyl)cycloheptimidazole (3.15 g, described in Example 2) and potassium carbonate (1.14 g) in dimethyl sulfoxide (10 ml) was stirred for 15 min and a solution of 2-propenyl bromide (1.18 g) in dimethyl sulfoxide was added. The reaction mixture was stirred for 2.5 hr and diluted with brine. The solution was extracted with ethyl acetate and the organic extract was dried and evaporated to give the title compound (1.8 g): mp 108°-111° C.; ir(CHCl3) 1600, 1565 and 1520 cm-1 ; uv max (MeOH) 263(ε29,965), 237(ε25,490) and 362 nm (ε21,620) and nmr(CDCl3)δ 2.6(4H,s), 3.0(2H,d), 4.05(4H,t), 5.15(2H,m), 5.75(1H,m) and 7.65(5H,m).

後処理

  1. stirringThe reaction mixture was stirred for 2.5 hr
  2. extractionThe solution was extracted with ethyl acetate
  3. extractionthe organic extract
  4. customwas dried
  5. customevaporated

出典と根拠

ORDレコード
ord-6ac9863b3c254022abed5e08ed686052
出典データセット
uspto-grants-1981_03
特許番号
US04258188

反応ノート

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