ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Methanol → N-(2-methylphenyl)butanamide

HRID 1168003
ノート
印刷プレビュー

反応式

HRID 1168003 の反応式
[NH2:1][C:2]1[C:3]([CH3:8])=[CH:4][CH:5]=[CH:6][CH:7]=1.[C:9](Cl)(=[O:13])[CH2:10][CH2:11][CH3:12].CO>C1(C)C=CC=CC=1>[CH3:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[NH:1][C:9](=[O:13])[CH2:10][CH2:11][CH3:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 7242O-ToluidineHCID 8855Butyryl chloride

生成物 1

HCID 221809N-(2-methylphenyl)butanamide収率 92%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

1128.6 g of o-toluidine were initially charged in 500 ml of toluene and heated to 90° C. 134.3 g of butyryl chloride were added dropwise within 2 hours. After completed addition, the mixture was heated to reflux and stirring continued at this temperature until the end of gas formation. The mixture was cooled to 70° C., 12 ml of methanol were added and stirring was continued for an hour. To remove the methanol, the mixture was heated and 70 ml were distilled off. 300 ml of toluene were then distilled off and 400 ml of cyclohexane were added. The mixture was cooled to 10° C. and filtration gave 199.5 g (92% yield) of the product in 98% purity after drying.

後処理

  1. additionaddition
  2. temperaturethe mixture was heated
  3. temperatureto reflux
  4. temperatureThe mixture was cooled to 70° C.
  5. stirringstirring
  6. waitwas continued for an hour
  7. customTo remove the methanol
  8. temperaturethe mixture was heated
  9. distillation70 ml were distilled off
  10. distillation300 ml of toluene were then distilled off
  11. addition400 ml of cyclohexane were added
  12. temperatureThe mixture was cooled to 10° C.
  13. filtrationfiltration

出典と根拠

ORDレコード
ord-e73b5b86e610472dba0d7db5bf73728e
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06620962B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート