Dicyclohexylcarbodiimide → HCID 18183268, 화합물

HRID 1359512노트

반응식

HRID 1359512 반응식
[Br:1][CH:2]([CH3:6])[C:3](O)=[O:4].[CH3:7][NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[F:15].C1(N=C=NC2CCCCC2)CCCCC1>C(Cl)(Cl)Cl>[F:15][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[N:8]([CH3:7])[C:3](=[O:4])[CH:2]([Br:1])[CH3:6]

참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 117292-Bromopropionic acidHCID 27590102-Fluoro-N-methylaniline

생성물 1

HCID 18183268HCID 18183268, 화합물수율 87.4%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

반응 조건

온도
0 °C

실험 절차

2-Bromopropionic acid (3.4 g, 0.022 mol) and N-methyl-2-fluoroaniline(3 g. 0.024 mol) were dissolved in 50 ml of chloroform and cooled to 0° C. A solution of dicyclohexylcarbodiimide(5 g, 0.024 mol) in 10 ml of chloroform was slowly injected through a syringe. A temperature of the reaction mixture was raised to room temperature and it was stirred for 1 hour. Solid remained during the reaction was filtered out and washed twice with 20 ml of chloroform. The filtrate was concentrated under reduced pressure and the crude product was purified by column chromatography (eluent; ethyl acetate/n-hexane=⅓) to afford 5 g of the target product.

후처리

  1. temperatureA temperature of the reaction mixture was raised to room temperature
  2. filtrationwas filtered out
  3. washwashed twice with 20 ml of chloroform
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe crude product was purified by column chromatography (eluent; ethyl acetate/n-hexane=⅓)

출처 및 근거

ORD 기록
ord-b314bd09a9f24468856754cbfdf52ad4
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06600048B2

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