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Hydrochloric Acid → HCID 20043928, 화합물

HRID 1761318
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HRID 1761318 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric Acid2회HCID 13557219HCID 13557219, 화합물

생성물 1

HCID 20043928HCID 20043928, 화합물수율 146%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-91a5319e2f444893aa50258899d5885f
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04826527

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