Phosgene → HCID 18965182, 화합물

HRID 486752노트

반응식

HRID 486752 반응식
[CH:1]1[CH:6]=[CH:5][C:4]([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Br:14])[CH:9]=2)=[CH:3][CH:2]=1.[C:15](Cl)([Cl:17])=[O:16].CCCCCC.C(OCC)(=O)C>C1(C)C=CC=CC=1>[Br:14][C:10]1[CH:9]=[C:8]([N:7]([C:4]2[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=2)[C:15]([Cl:17])=[O:16])[CH:13]=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 6371PhosgeneHCID 149586063-BromodiphenylamineHCID 21226206Ethyl acetate hexane

생성물 1

HCID 18965182HCID 18965182, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
90 °C

실험 절차

A solution of 15.0 g (60.4 mmole) of 3-bromodiphenylamine [i.e., N-(3-bromophenyl)aniline] [S. Kurzepa and J. Cieslak, Roczniki Chem., 34, 111 (1960)] in 30 ml of toluene and 50 ml (116 mmole) of 1.93M phosgene in toluene were combined and heated at 90° C. under nitrogen for 2 hours with stirring. The red orange colored solution was cooled, flushed with nitrogen for 2 hours to remove excess Phosgene and concentrated in vacuo to 18.0 g (58.0 mmole, 96%) of red orange oil which was homogeneous by TLC (4:1 hexane-ethyl acetate, Rf =0.80).

후처리

  1. temperatureThe red orange colored solution was cooled
  2. customflushed with nitrogen for 2 hours
  3. customto remove excess Phosgene

출처 및 근거

ORD 기록
ord-607c8589fd264ac498f6637306d4054f
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292726

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