Phenyl isocyanate → Pencycuron

HRID 1704751

反応式

HRID 1704751 の反応式
[C:1]1([N:7]=[C:8]=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:10][C:11]1[CH:23]=[CH:22][C:14]([CH2:15][NH:16][CH:17]2[CH2:21][CH2:20][CH2:19][CH2:18]2)=[CH:13][CH:12]=1>CCCCCC>[Cl:10][C:11]1[CH:12]=[CH:13][C:14]([CH2:15][N:16]([CH:17]2[CH2:21][CH2:20][CH2:19][CH2:18]2)[C:8]([NH:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[O:9])=[CH:22][CH:23]=1

参加物

4

反応物 2

HCID 7672Phenyl isocyanateHCID 8340834-Chloro-N-cyclopentylbenzylamine

生成物 1

HCID 91692Pencycuron収率 95%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒2 回

実験手順

A solution of 12 grams (0.1 mole) of phenylisocyanate in 50 ml of hexane was added dropwise to 21 grams (0.1 mole) of N-4-chlorobenzyl-N-cyclopentylamine in 400 ml of hexane under cooling and stirring conditions. After the addition, the temperature of the reaction mixture was gradually raised, and the solution was then stirred at 50° C. for about 7 hours. The mixture was cooled and filtered. The residue was recrystallized from a mixed solvent of hexane-ethyl alcohol. 31 grams of N-4-chlorobenzyl-N-cyclopentyl-N'-phenylurea were obtained. Yield: 95%. Melting point: 129°-134° C.

後処理

  1. temperatureunder cooling
  2. additionAfter the addition
  3. temperaturethe temperature of the reaction mixture was gradually raised
  4. stirringthe solution was then stirred at 50° C. for about 7 hours
  5. temperatureThe mixture was cooled
  6. filtrationfiltered
  7. customThe residue was recrystallized from a mixed solvent of hexane-ethyl alcohol

出典と根拠

ORDレコード
ord-3135366f812149b0991e7679a9603783
出典データセット
uspto-grants-1978_11
特許番号
US04127673

関連ノート

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