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Sodium Bicarbonate → [4-(2,4-Dimethylphenyl)piperazin-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-2-hydroxyphenyl]methanone

HRID 2411502
ノート
印刷プレビュー

反応式

HRID 2411502 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[N:9]1[CH2:14][CH2:13][N:12]([C:15]([C:17]2[CH:22]=[CH:21][C:20]([N:23]3[CH2:27][CH2:26][CH2:25][S:24]3(=[O:29])=[O:28])=[CH:19][C:18]=2[O:30]C)=[O:16])[CH2:11][CH2:10]1.ClCCl.B(Br)(Br)Br.C(=O)([O-])O.[Na+]>ClCCl>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[N:9]1[CH2:10][CH2:11][N:12]([C:15]([C:17]2[CH:22]=[CH:21][C:20]([N:23]3[CH2:27][CH2:26][CH2:25][S:24]3(=[O:29])=[O:28])=[CH:19][C:18]=2[OH:30])=[O:16])[CH2:13][CH2:14]1
参加物反応条件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 516892Sodium BicarbonateHCID 22277759Boron tribromide dichloromethaneHCID 71252392[4-(2,4-Dimethylphenyl)piperazin-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-2-methoxyphenyl]methanone

生成物 1

HCID 71252235[4-(2,4-Dimethylphenyl)piperazin-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-2-hydroxyphenyl]methanone収率 49.6%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

反応条件

温度
-78 °C

実験手順

[4-(2,4-Dimethylphenyl)piperazin-1-yl][4-(1,1-dioxo-1λ6-isothiazolidin-2-yl)-2-methoxyphenyl]methanone (0.35 g) described in Example 89 was dissolved in dichloromethane (20 mL), 1 mol/L boron tribromide dichloromethane solution (4 mL) was added while stirring at −78° C. under cooling, and the mixture was stirred while rising the temperature to room temperature. Into the reaction mixture was poured ice water, and the mixture was neutralized with sodium hydrogen carbonate and extracted with chloroform. The organic layer was washed with saturated brine, and the solvent was evaporated. The obtained residue was purified by column chromatography (chloroform:methanol) to give the title compound (168 mg).

後処理

  1. temperatureunder cooling
  2. stirringthe mixture was stirred
  3. customto room temperature
  4. extractionextracted with chloroform
  5. washThe organic layer was washed with saturated brine
  6. customthe solvent was evaporated
  7. customThe obtained residue was purified by column chromatography (chloroform:methanol)

出典と根拠

ORDレコード
ord-6d218dde807f4680835bb95e02bdcc2e
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08816079B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート