Triethylamine → HCID 20467443、化合物

HRID 1903562ノート

反応式

HRID 1903562 の反応式
[CH2:1]([C:3]1[NH:4][CH:5]=[C:6]([CH3:8])[N:7]=1)[CH3:2].C(N(CC)CC)C.[Cl:16][C:17]1[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[C:18]=1[C:19](Cl)=[O:20]>O1CCCC1.Cl.C(N(CC)CC)C>[Cl:16][C:17]1[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[C:18]=1[C:19]([N:4]1[CH:5]=[C:6]([CH3:8])[N:7]=[C:3]1[CH2:1][CH3:2])=[O:20]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 22596843HCID 22596843、化合物HCID 178437635HCID 178437635、化合物

生成物 1

HCID 20467443HCID 20467443、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 11130Triethylamine hydrochloride溶媒

実験手順

15.4 g of 2-ethyl-4-methyl-imidazole are dissolved in 100 ml of tetrahydrofuran; 14.6 g of triethylamine are added, and there can then added dropwise, within 30 minutes at reflux temperature, 30.8 g of 2-chloro-6-nitrobenzoyl chloride, dissolved in 50 ml of tetrahydrofuran, in the process of which triethylamine hydrochloride precipitates. After 3 hours of refluxing, the mixture is filtered with suction, and the solvent is removed in the rotary evaporator. Recrystallisation of the residue from 85 ml of toluene yields 27.7 g (67.3% of theory) of the desired product, m.p. 119°-120° C.

後処理

  1. additionthere can then added dropwise, within 30 minutes
  2. customprecipitates
  3. temperatureAfter 3 hours of refluxing
  4. filtrationthe mixture is filtered with suction
  5. customthe solvent is removed in the rotary evaporator
  6. customRecrystallisation of the residue from 85 ml of toluene

出典と根拠

ORDレコード
ord-9a2acad788a645d38dc13b894e906a3e
出典データセット
uspto-grants-1984_03
特許番号
US04436892

反応ノート

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