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Trifluoroacetic acid → HCID 53913605、化合物

HRID 849853
ノート
印刷プレビュー

反応式

HRID 849853 の反応式
C(O[C:6](=O)[N:7]([C@@H:9]([C:17]1[O:18][C:19]([C:22](=[O:24])[NH2:23])=[N:20][N:21]=1)[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)C)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH3:6][NH:7][C@@H:9]([C:17]1[O:18][C:19]([C:22]([NH2:23])=[O:24])=[N:20][N:21]=1)[CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH: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

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 53673637HCID 53673637、化合物

生成物 1

HCID 53913605HCID 53913605、化合物収率 99.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

((1R)-1-(5-Carbamoyl-[1,3,4]oxadiazol-2-yl)-2-phenylethyl)methylcarbamic acid tert-butylester (350 mg, 1.01 mmol) was dissolved in dichloromethane (6 ml). The solution was cooled to 0° C. Trifluoroacetic acid (2 ml) was added dropwise. The solution was stirred for 30 min. The solvent was removed in vacuo. The residue was dissolved in dichloromethane (6 ml) and the solvent was removed in vacuo. The residue was again dissolved in dichloromethane (6 ml) and the solvent was removed in vacuo. The residue was dissolved in dichloromethane (10 ml). This phase was washed with water. The aqueous phase was lyophilized to give 247 mg of crude 5-((1R)-1-methylamino-2-phenylethyl)-[1,3,4]oxadiazole-2-carboxylic acid amide, which was used for the further synthesis.

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionThe residue was dissolved in dichloromethane (6 ml)
  3. customthe solvent was removed in vacuo
  4. dissolutionThe residue was again dissolved in dichloromethane (6 ml)
  5. customthe solvent was removed in vacuo
  6. dissolutionThe residue was dissolved in dichloromethane (10 ml)
  7. washThis phase was washed with water

出典と根拠

ORDレコード
ord-f57262415a9d4178a6a87922e1d2cb38
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06013658

反応ノート

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