Hexane → HCID 70816656, 화합물

HRID 1887789

반응식

HRID 1887789 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:11])[CH2:9][CH3:10])=[C:4]([NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:3]=1.Cl[C:20](=[O:25])[C:21]([O:23][CH3:24])=[O:22].CCCCCC.C(OCC)(=O)C>C1(C)C=CC=CC=1>[CH3:24][O:23][C:21](=[O:22])[C:20]([N:12]([C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[CH:6][C:5]=1[C:8](=[O:11])[CH2:9][CH3:10])[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)=[O:25]

참가 물질

6

반응물 4

HCID 8058HexaneHCID 8857Ethyl AcetateHCID 79846Methyl chloroglyoxylateHCID 708166141-(4-Chloro-2-phenylamino-phenyl)-propan-1-one

생성물 1

HCID 70816656HCID 70816656, 화합물수율 87.6%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
110 °C

실험 절차

To a solution of 1-(4-chloro-2-phenylamino-phenyl)-propan-1-one (13.0 g, 50.2 mmol) in toluene (150 mL) was added methyl chlorooxoacetate (42.86 g, 350.0 mmol) at room temperature under nitrogen. The reaction mixture was heated at reflux at 110° C. for 16 hr. Completion of the reaction was monitored by silica TLC (mobile phase; hexane:ethyl acetate=1:1; Rf=0.5). The reaction mixture was concentrated under vacuum to afford 15.2 g (87.6% crude yield) of N-(5-chloro-2-propionyl-phenyl)-N-phenyl-oxalamic acid methyl ester. The crude product was used in the next step without further purification.

후처리

  1. temperatureThe reaction mixture was heated
  2. concentrationThe reaction mixture was concentrated under vacuum

출처 및 근거

ORD 기록
ord-d8fb32f5730d4ecaa7e2e137302bf31b
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501732B2

연결된 노트

불러오는 중…