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2-Chlorobenzoyl isocyanate → 1-(2-Chlorobenzoyl)-3-[2,5-dimethyl-3-chloro-4-(2-chloro-4-phenylphenoxy) phenyl]urea

HRID 980567
ノート
印刷プレビュー

反応式

HRID 980567 の反応式
[Cl:1][C:2]1[CH:18]=[C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:16]=[CH:15][C:3]=1[O:4][C:5]1[C:11]([CH3:12])=[CH:10][C:8]([NH2:9])=[C:7]([CH3:13])[C:6]=1[Cl:14].[Cl:25][C:26]1[CH:36]=[CH:35][CH:34]=[CH:33][C:27]=1[C:28]([N:30]=[C:31]=[O:32])=[O:29]>C1(C)C=CC=CC=1.CCCCCC>[Cl:25][C:26]1[CH:36]=[CH:35][CH:34]=[CH:33][C:27]=1[C:28]([NH:30][C:31]([NH:9][C:8]1[CH:10]=[C:11]([CH3:12])[C:5]([O:4][C:3]2[CH:15]=[CH:16][C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:18][C:2]=2[Cl:1])=[C:6]([Cl:14])[C:7]=1[CH3:13])=[O:32])=[O:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 99423112-Chlorobenzoyl isocyanateHCID 137729294-(2-Chloro-4-phenylphenoxy)-2,5-dimethyl-3-chloroaniline

生成物 1

HCID 137729301-(2-Chlorobenzoyl)-3-[2,5-dimethyl-3-chloro-4-(2-chloro-4-phenylphenoxy) phenyl]urea

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒3 回HCID 8058Hexane溶媒

実験手順

To a solution containing 1.61 grams (0.004 moles) of 4-(2-chloro-4-phenylphenoxy)-2,5-dimethyl-3-chloroaniline prepared in Part B and 3 milliliters of toluene, which solution was warmed to 40° C.-50° C. and placed under an atmosphere of nitrogen, was added a solution containing 0.98 grams (0.005 moles) of 2-chlorobenzoyl isocyanate and 0.05 milliliters of toluene. The resulting mixture was then heated to a temperature of 60° C.-70° C, for a period of 0.5-1.0 hours. After cooling to ambient temperature, the reaction mixture was diluted with 4 milliliters of toluene and 2 milliliters of hexane. This mixture was then filtred to give a solid material. The solid material was washed once with a toluene-hexane mixture (1:2 volume ratio) and finally once with hexane and then dried overnight in a vaccum oven at 50° C. This afforded a tan powder material having a melting point of 198° C.-199° C. Elemental analysis of the tan powder indicated the following:

後処理

  1. temperaturewas warmed to 40° C.-50° C.
  2. additionwas added a solution
  3. temperatureThe resulting mixture was then heated to a temperature of 60° C.-70° C, for a period of 0.5-1.0 hours
  4. customto give a solid material
  5. washThe solid material was washed once with a toluene-hexane mixture (1:2 volume ratio) and finally once with hexane
  6. customdried overnight in a vaccum oven at 50° C
  7. customThis afforded a tan powder material

出典と根拠

ORDレコード
ord-dab7383a53d74a53ae2023c93ef92d64
出典データセット
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04638088

反応ノート

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