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Diphosgene → 2-Methyl-5-phenylbenzylisocyanate

HRID 1883633
ノート
印刷プレビュー

反応式

HRID 1883633 の反応式
O=C(Cl)[O:3][C:4](Cl)(Cl)Cl.[CH3:9][C:10]1[CH:17]=[CH:16][C:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:14][C:11]=1[CH2:12][NH2:13]>C1(C)C=CC=CC=1>[CH3:9][C:10]1[CH:17]=[CH:16][C:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:14][C:11]=1[CH2:12][N:13]=[C:4]=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10426DiphosgeneHCID 235082132-Methyl-5-phenylbenzylamine

生成物 1

HCID 120565262-Methyl-5-phenylbenzylisocyanate収率 99.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

2.5 g (12.6 mmol) of diphosgene, 0.40 g of activated carbon and 30 ml of toluene were mixed, and allowed to left overnight, and to this solution was slowly dropped at room temperature a solution prepared by dissolving 1.00 g (5.07 mmol) of 2-methyl-5-phenylbenzylamine (produced in the same manner as in Intermediate Production Example 6) in 5 ml of toluene. The reaction mixture turned to white suspension directly after the dropping. The white suspension was stirred at room temperature for 1 hour, further stirred for 5 hours under reflux with heating, then, concentrated under reduced pressure to obtain 1.13 g of 2-methyl-5-phenybenzyl isocyanate.

後処理

  1. additionto this solution was slowly dropped at room temperature a solution
  2. customprepared
  3. stirringfurther stirred for 5 hours
  4. temperatureunder reflux
  5. temperaturewith heating
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-26cce3656c6f4abc91eef67c2c7d5502
出典データセット
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06762197B2

反応ノート

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