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Hydrochloric Acid → HCID 20043928、化合物

HRID 1761318
ノート
印刷プレビュー

反応式

HRID 1761318 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]2[C:13](=[O:14])[C:12]([CH3:16])([CH3:15])[CH2:11][O:10]2)=[C:4]([Cl:17])[CH:3]=1.Cl>CO>[ClH:17].[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]2[C:13](=[O:14])[C:12]([CH3:15])([CH3:16])[CH2:11][O:10]2)=[C:4]([Cl:17])[CH:3]=1
参加物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 313Hydrochloric Acid2 回HCID 13557219HCID 13557219、化合物

生成物 1

HCID 20043928HCID 20043928、化合物収率 146%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2.0 grams (0.008 mole) of 2-[(4-amino-2-chlorophenyl)methyl]-4,4-dimethyl-3-isoxazolidinone in 25 mL of methanol was stirred, and 0.78 gram (0.008 mole) of concentrated hydrochloric acid was added dropwise. Upon completion of addition the reaction mixture was stirred for 20 minutes. Analysis of the reaction mixture by thin layer chromatography (TLC) indicated the presence of unreacted amine. An additional 0.5 gram of concentrated hydrochloric acid was added, and the reaction mixture was stirred for 30 minutes more. The reaction mixture was concentrated under reduced pressure to a residue. The residue was dissolved in 20 mL of ethanol. A solid was precipitated from the solution by the addition of 20 mL of diethyl ether. The solid was collected by filtration and was dried to yield 1.7 grams of 2-[(4-amino-2-chlorophenyl)methyl]-4,4-dimethyl-3-isoxazolidinone hydrochloride as a solid.

後処理

  1. additionUpon completion of addition the reaction mixture
  2. stirringthe reaction mixture was stirred for 30 minutes more
  3. concentrationThe reaction mixture was concentrated under reduced pressure to a residue
  4. dissolutionThe residue was dissolved in 20 mL of ethanol
  5. customA solid was precipitated from the solution by the addition of 20 mL of diethyl ether
  6. filtrationThe solid was collected by filtration
  7. customwas dried

出典と根拠

ORDレコード
ord-91a5319e2f444893aa50258899d5885f
出典データセット
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04826527

反応ノート

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