Hydrochloric Acid → 1-[3-(4-Chlorophenyl)-1,2-oxazol-5-yl]methanamine

HRID 2420122ノート

反応式

HRID 2420122 の反応式
[Br-].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:13]=[C:12]([CH2:14][N+:15]34CN5CN(CN(C5)C3)C4)[O:11][N:10]=2)=[CH:5][CH:4]=1.Cl>CO>[NH2:15][CH2:14][C:12]1[O:11][N:10]=[C:9]([C:6]2[CH:7]=[CH:8][C:3]([Cl:2])=[CH:4][CH:5]=2)[CH:13]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 20339738HCID 20339738、化合物

生成物 1

HCID 27641631-[3-(4-Chlorophenyl)-1,2-oxazol-5-yl]methanamine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 205 g. portion of the product of Example 5 was dissolved in 1.5 l. of methanol and 250 ml. of concentrated hydrochloric acid was added. The mixture was stirred at reflux temperature overnight, and the solvent was then evaporated under vacuum. The residue was neutralized with aqueous sodium hydroxide and the product was extracted from the aqueous mixture with methylene dichloride and was purified by evaporating the solvent and recrystallizing the residue from ethanol-petroleum ether. The product was 78 g. of 5-aminomethyl-3-(4-chlorophenyl)isoxazole, m.p. 81°.

後処理

  1. temperatureat reflux temperature overnight
  2. customthe solvent was then evaporated under vacuum
  3. extractionthe product was extracted from the aqueous mixture with methylene dichloride
  4. customwas purified
  5. customby evaporating the solvent
  6. customrecrystallizing the residue from ethanol-petroleum ether

出典と根拠

ORDレコード
ord-bc52914786b947368ba3dfea748f34e5
出典データセット
uspto-grants-1978_08
特許番号
US04109002

反応ノート

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