Phosgene → HCID 18965182、化合物

HRID 2226601ノート

反応式

HRID 2226601 の反応式
[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

参加物

5

反応物 3

HCID 6371PhosgeneHCID 149586063-BromodiphenylamineHCID 21226206Ethyl acetate hexane

生成物 1

HCID 18965182HCID 18965182、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
90 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-ae12763054c04ea081bacff9e61871c1
出典データセット
uspto-grants-1994_09
特許番号
US05348955

反応ノート

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