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Water → HCID 13314712, 화합물

HRID 543572
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HRID 543572 반응식
[CH3:1][C:2]1([C:5]([OH:7])=O)[CH2:4][CH2:3]1.[Cl:8][C:9]1[CH:10]=[C:11]([CH:13]=[CH:14][C:15]=1[O:16][CH2:17][C:18]([F:21])([F:20])[F:19])[NH2:12].O>N1C=CC=CC=1>[Cl:8][C:9]1[CH:10]=[C:11]([NH:12][C:5]([C:2]2([CH3:1])[CH2:4][CH2:3]2)=[O:7])[CH:13]=[CH:14][C:15]=1[O:16][CH2:17][C:18]([F:20])([F:21])[F:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 813261-Methylcyclopropanecarboxylic acidHCID 133055253-Chloro-4-(2,2,2-trifluoroethoxy)aniline

생성물 1

HCID 13314712HCID 13314712, 화합물수율 82.9%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

To a solution of 1-methylcyclopropanecarboxylic acid (1.8 g) in pyridine (50 ml), a solution of 3-chloro-4-(2,2,2-trifluoroethoxy)aniline (2.3 g) in pyridine (10 ml) cooled with ice was dropwise added while stirring. After stirring at room temperature for 10 hours, the reaction mixture was admixed with water and extracted with ether. The extract was washed with 1 N hydrochloric acid, sodium hydrogen carbonate solution and saturated sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated. The crude crystals (2.8 g) were recrystallized from ethanol to give N-(3-chloro-4-(2,2,2-trifluoroethoxy)phenyl)-1-methylcyclopropanecarboxamide (2.6 g). M.P., 95°-96° C.

후처리

  1. additionwas dropwise added
  2. stirringAfter stirring at room temperature for 10 hours
  3. extractionextracted with ether
  4. washThe extract was washed with 1 N hydrochloric acid, sodium hydrogen carbonate solution and saturated sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe crude crystals (2.8 g) were recrystallized from ethanol

출처 및 근거

ORD 기록
ord-87150c4725c24e0a9f9f199c45308877
출처 데이터셋
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04447260

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