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Water → HCID 13557219, 화합물

HRID 1583481
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HRID 1583481 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([NH:8]C(OC(C)(C)C)=O)[CH:5]=[CH:4][C:3]=1[CH2:16][N:17]1[C:21](=[O:22])[C:20]([CH3:24])([CH3:23])[CH2:19][O:18]1.FC(F)(F)C(O)=O.O.C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl>[NH2:8][C:6]1[CH:5]=[CH:4][C:3]([CH2:16][N:17]2[C:21](=[O:22])[C:20]([CH3:23])([CH3:24])[CH2:19][O:18]2)=[C:2]([Cl:1])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 11430Potassium CarbonateHCID 13557261HCID 13557261, 화합물

생성물 1

HCID 13557219HCID 13557219, 화합물수율 85.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirred solution of 2.0 grams (0.006 mole) of 2-[2-chloro-4-(1,1-dimethylethoxycarbonylamino)phenyl]methyl-4,4-dimethyl-3-isoxazolidinone in 10 ml of methylene chloride was added dropwise a solution of 10 ml of trifluoroacetic acid in 10 ml of methylene chloride. Upon completion of addition the reaction mixture stirred at ambient temperature for 3.5 hours. The reaction mixture was slurried with 50 ml of water and neutralized with a saturated aqueous solution of potassium carbonate. A solid precipitate was collected by filtration to give 1.3 grams of 2-(4-amino-2-chlorophenyl)methyl-4,4-dimethyl-3-isoxazolidinone; m.p. 106°-108° C.

후처리

  1. additionUpon completion of addition the reaction mixture
  2. filtrationA solid precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-676246f099f04dd59fe27d9c3082f9a0
출처 데이터셋
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04552585

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