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Propargyl bromide → 1-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]-3-(2-propinyl)-1,3-dihydro-2H-benzimidazol-2-one

HRID 47519
ノート
印刷プレビュー

反応式

HRID 47519 の反応式
[CH3:1][O:2][C:3]([N:5]1[CH2:10][CH2:9][CH:8]([N:11]2[CH2:16][CH2:15][CH:14]([N:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[NH:19][C:18]3=[O:26])[CH2:13][CH2:12]2)[CH2:7][CH2:6]1)=[O:4].[H-].[Na+].[CH2:29](Br)[C:30]#[CH:31].C(=O)(O)[O-].[Na+]>CN(C)C=O.C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]([N:5]1[CH2:10][CH2:9][CH:8]([N:11]2[CH2:16][CH2:15][CH:14]([N:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[N:19]([CH2:31][C:30]#[CH:29])[C:18]3=[O:26])[CH2:13][CH2:12]2)[CH2:7][CH2:6]1)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7842Propargyl bromideHCID 24758Sodium hydrideHCID 516892Sodium Bicarbonate2 回HCID 227452181-[1-(1-methoxycarbonylpiperidin-4-yl)piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one

生成物 1

HCID 121276521-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]-3-(2-propinyl)-1,3-dihydro-2H-benzimidazol-2-one

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒
HCID 6228Dimethylformamide溶媒

実験手順

1-[1-(1-Methoxycarbonylpiperidin-4-yl)piperidin-4-yl]-1,3-di-hydro-2H-benzimidazol-2-one (28 mg) as synthesized by the method of Referential Example 1 was dissolved in 5 ml of dimethylformamide, and to which 2.0 mg of sodium hydride was added under cooling with ice, followed by 30 minutes' stirring. Ten(10) mg of propargyl bromide was added to the reaction liquid which was stirred for further 3 hours at room temperature. After adding saturated aqueous sodium bicarbonate solution and concentrating the reaction liquid, the resulting residue was distributed between saturated aqueous sodium bicarbonate solution and chloroform. The organic layer was dried over anhydrous sodium sulfate, concentrated, and the resulting residue was purified by silica gel column chromatography (chloroform/methanol=20/1). Thus 11.3 mg of the title compound was obtained as a colorless oil.

後処理

  1. temperatureunder cooling with ice
  2. stirringwas stirred for further 3 hours at room temperature
  3. concentrationconcentrating
  4. customthe reaction liquid
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol=20/1)

出典と根拠

ORDレコード
ord-dd75cdfd697344ccab8f96882d9483e6
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06699880B1

反応ノート

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