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Water → 5-Chloro-2-(1-piperidyl)benzooxazole

HRID 378880
ノート
印刷プレビュー

反応式

HRID 378880 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[OH:9].[NH:10]1[CH2:15][CH2:14][CH:13](C(O)=O)[CH2:12][CH2:11]1.O.[OH-].[K+].[C:22]1(C)C(C)=CC=CC=1>>[Cl:8][C:6]1[CH:5]=[CH:4][C:3]2[O:9][C:22]([N:10]3[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]3)=[N:1][C:2]=2[CH:7]=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

6

反応物 5

HCID 962WaterHCID 37734-Piperidinecarboxylic acidHCID 7237O-XyleneHCID 72652-Amino-4-chlorophenolHCID 14797Potassium Hydroxide

生成物 1

HCID 2302965-Chloro-2-(1-piperidyl)benzooxazole

反応条件

温度
180 °C

実験手順

2-Amino-4-chlorophenol (400 mg) and 4-piperidinecarboxylic acid (360 mg) were mixed with polyphosphate (2 g) in xylene (30 ml) and stirred with heating at 180° C. for 2 hours. After cooling to room temperature, the reaction was stopped by adding water. The filtrate was adjusted to pH 12 with 50% potassium hydroxide aqueous solution and extracted with methylene chloride. The organic layer was washed with saturated brine and dried with magnesium sulfate, and then the solvent was evaporated under a reduced pressure to obtain the title compound 5-chloro-2-(1-piperidyl)benzoxazole (218 mg).

後処理

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with methylene chloride
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried with magnesium sulfate
  5. customthe solvent was evaporated under a reduced pressure

出典と根拠

ORDレコード
ord-00dc604feb474552bf099ec19e5774d3
出典データセット
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06297246B1

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