1,2-Diaminocyclohexane → 4-[(2-Amino)cyclohexylamino]-2,5,6-trichloro-1,3-dicyanobenzene

HRID 2304945

反応式

HRID 2304945 の反応式
[Cl:1][C:2]1[C:7]([C:8]#[N:9])=[C:6](Cl)[C:5]([Cl:11])=[C:4]([Cl:12])[C:3]=1[C:13]#[N:14].[NH2:15][CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH:17]1[NH2:22]>C(#N)C>[NH2:15][CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH:17]1[NH:22][C:6]1[C:5]([Cl:11])=[C:4]([Cl:12])[C:3]([C:13]#[N:14])=[C:2]([Cl:1])[C:7]=1[C:8]#[N:9]

参加物

4

反応物 2

HCID 46101,2-DiaminocyclohexaneHCID 15910Chlorothalonil

生成物 1

HCID 222229614-[(2-Amino)cyclohexylamino]-2,5,6-trichloro-1,3-dicyanobenzene収率 90%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To the slurry of 2,4,5,6-tetrachloro-1,3-dicyanobenzene (2.0 g, 7.5 mmol) in acetonitrile (40 ml) triethylamine (5.0 ml) is added, then 1,2-diaminocyclohexane (0.86 g, 7.5 mmol) and the reaction mixture is heated under reflux for 1 h. It is cooled to ambient temperature, then deposited on ice for few hours, and the crystalline product is collected on filter. 2.32 g (89%) of the title product as pale-yellow powder are obtained.

後処理

  1. temperatureunder reflux for 1 h
  2. waitdeposited on ice for few hours
  3. customthe crystalline product is collected
  4. filtrationon filter

出典と根拠

ORDレコード
ord-2d9c4f4a4b5349e1938ee389dde22d99
出典データセット
uspto-grants-2002_08
特許番号
US06437167B1

関連ノート

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