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Potassium Carbonate → HCID 178492556、化合物

HRID 710059
ノート
印刷プレビュー

反応式

HRID 710059 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][C:12]=1[O:13][CH3:14])[O:6][CH2:7][C:8]#[N:9].[NH:15]([C:17]([C@@H:19]1[CH2:23][CH2:22][CH2:21][N:20]1[C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])=O)[NH2:16].C([O-])([O-])=O.[K+].[K+]>C(O)CCC>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][C:12]=1[O:13][CH3:14])[O:6][CH2:7][C:8]1[NH:9][C:17]([C@@H:19]2[CH2:23][CH2:22][CH2:21][N:20]2[C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])=[N:15][N:16]=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 11430Potassium CarbonateHCID 10014050tert-Butyl (2S)-2-(hydrazinecarbonyl)pyrrolidine-1-carboxylateHCID 189913533,4-Dimethoxyphenoxyacetonitrile

生成物 1

HCID 178492556HCID 178492556、化合物収率 31.9%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
160 °C

実験手順

To a n-butanol (10 ml) solution of 2-(3,4-dimethoxyphenoxy)acetonitrile (1.26 g) and (S)-t-butyl 2-(hydrazinecarbonyl)pyrrolidine-1-carboxylate (500 mg), K2CO3 (150 mg) was added. The resulting mixture was stirred at 160° C. for an hour under microwave irradiation. After distilling off the solvent under reduced pressure, water was added, followed by extraction with ethyl acetate. After distilling off the solvent under reduced pressure, the residue was purified by silica gel chromatography and NH-form silica gel chromatography to give the titled compound (281 mg).

後処理

  1. distillationAfter distilling off the solvent under reduced pressure, water
  2. additionwas added
  3. extractionfollowed by extraction with ethyl acetate
  4. distillationAfter distilling off the solvent under reduced pressure
  5. customthe residue was purified by silica gel chromatography and NH-form silica gel chromatography

出典と根拠

ORDレコード
ord-0a0cbec2585c43d78f9151704aaf8d69
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181229B2

反応ノート

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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