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

Acetic Acid → 2,5-Dimethyl-3-nitrobenzaldehyde

HRID 2286457
ノート
印刷プレビュー

反応式

HRID 2286457 の反応式
[CH3:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][C:7]([CH3:13])=[CH:6][C:3]=1[CH2:4]Cl.C(O)(=[O:16])C.C1N2CN3CN(C2)CN1C3.Cl>O>[CH3:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][C:7]([CH3:13])=[CH:6][C:3]=1[CH:4]=[O:16]
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

6

反応物 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 4101HexamethylenetetramineHCID 156185981-(Chloromethyl)-2,5-dimethyl-3-nitrobenzene

生成物 1

HCID 128316812,5-Dimethyl-3-nitrobenzaldehyde収率 53%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

The mixture constituted by 2,5-dimethyl-3-nitrobenzyl-chloride (A) prepared according to M. J. WINCHESTER and F. D. POPP, J. Het. Chem. 12, p. 547 (1975) (610 g), acetic acid (1280 ml, water (1280 ml) and hexamethylene tetramine (855 g) was heated with reflux under stirring for 2 hours. 1037 ml of concentrated hydrochloric acid were then added in 10 minutes and the mixture was again heated with reflux for 20 minutes. This mixture, cooled to 0° C., gave a solid which was filtered off, dried and recrystallised from cyclohexane (4 liters) to give 290.5 g (53%) of yellow needles corresponding to the aldehyde of formula B, melting point : =90°-93° C.

後処理

  1. customprepared
  2. temperaturewith reflux
  3. temperaturethe mixture was again heated
  4. temperaturewith reflux for 20 minutes
  5. customgave a solid which
  6. filtrationwas filtered off
  7. customdried
  8. customrecrystallised from cyclohexane (4 liters)

出典と根拠

ORDレコード
ord-b2747e11718f43fe9dff187489b3fef4
出典データセット
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04266060

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