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2-Chloroethyl chloroformate → 2-(5-Phenyl-1,2,4-oxadiazol-3-yl)morpholine hydrochloride

HRID 2063356
ノート
印刷プレビュー

反応式

HRID 2063356 の反応式
C([N:8]1[CH2:13][CH2:12][O:11][CH:10]([C:14]2[N:18]=[C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[O:16][N:15]=2)[CH2:9]1)C1C=CC=CC=1.[Cl:25]C(OCCCl)=O>ClCCCl>[ClH:25].[C:19]1([C:17]2[O:16][N:15]=[C:14]([CH:10]3[O:11][CH2:12][CH2:13][NH:8][CH2:9]3)[N:18]=2)[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=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 123052-Chloroethyl chloroformateHCID 580978824-Benzyl-2-(5-phenyl-1,2,4-oxadiazol-3-yl)morpholine2 回

生成物 1

HCID 668424982-(5-Phenyl-1,2,4-oxadiazol-3-yl)morpholine hydrochloride

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
70 °C

実験手順

To a stirred solution of 4-benzyl-2-(5-phenyl-1,2,4-oxadiazol-3-yl)morpholine (intermediate 27, 900 mg, 2.80 mmol) in 1,2-dichloroethane (2.0 ml) was added chloroethyl chloroformate (0.46 ml, 4.20 mmol), and the reaction mixture was stirred at 70° C. for 4 hours. The reaction mixture was concentrated in vacuo. After removal of the solvent, the residue was dissolved in methanol (2.0 ml), and the solution was stirred under reflux for one hour. When the reaction was complete (checked by thin layer chromatography), the reaction mixture was concentrated in vacuo. The resulting 2-(5-phenyl-[1,2,4]oxadiazol-3-yl)-morpholine hydrochloride (intermediate 28) was used for next reaction without further purification.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customAfter removal of the solvent
  3. dissolutionthe residue was dissolved in methanol (2.0 ml)
  4. stirringthe solution was stirred
  5. temperatureunder reflux for one hour
  6. concentrationthe reaction mixture was concentrated in vacuo
  7. customThe resulting 2-(5-phenyl-[1,2,4]oxadiazol-3-yl)-morpholine hydrochloride (intermediate 28) was used for next reaction without further purification

出典と根拠

ORDレコード
ord-474c773cf3eb4410920469d20b88634b
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08288383B2

反応ノート

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