Potassium Carbonate → 1260081-94-4

HRID 1533902ノート

反応式

HRID 1533902 の反応式
Cl.[Cl:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7]Cl.[CH2:9]([C:11]1[CH:12]=[C:13]([CH:15]=[CH:16][CH:17]=1)[NH2:14])[CH3:10].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[ClH:2].[CH2:9]([C:11]1[CH:12]=[C:13]([N:14]2[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]2)[CH:15]=[CH:16][CH:17]=1)[CH3:10]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 114753-EthylanilineHCID 522769Bis(2-chloroethyl)amine hydrochloride

生成物 1

HCID 199114721260081-94-4収率 71%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 73.3 g (0.411 mol) of bis(2-chloroethyl)amine hydrochloride and 49.7 g (0.411 mol) of 3-ethylaniline in 500 mL of absolute ethanol was heated at reflux for 16 h under a nitrogen atmosphere. The mixture was cooled and 85.2 g (0.617 mol) of anhydrous potassium carbonate was added and heating was continued for 16 h. The hot mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was triturated with ethyl acetate to yield 65.7 g (71%) of solid. A portion of this crude product was recrystallized from 2-propanol to yield a white crystalline solid, mp 194°-195° C.

後処理

  1. temperatureat reflux for 16 h under a nitrogen atmosphere
  2. temperatureThe mixture was cooled
  3. temperatureheating
  4. filtrationThe hot mixture was filtered
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was triturated with ethyl acetate

出典と根拠

ORDレコード
ord-4814a6080f1847609583721c1430c5a0
出典データセット
uspto-grants-1992_02
特許番号
US05086055

反応ノート

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