Triethylamine → N-(2-Chloropropyl)-N,2,6-trimethylbenzenamine

HRID 1649976노트

반응식

HRID 1649976 반응식
CS([Cl:5])(=O)=O.[CH3:6][N:7]([CH2:16][CH:17](O)[CH3:18])[C:8]1[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:15].C(N(CC)CC)C>ClCCCl>[CH3:6][N:7]([CH2:16][CH:17]([Cl:5])[CH3:18])[C:8]1[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:15]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 13674770HCID 13674770, 화합물

생성물 1

HCID 13674775N-(2-Chloropropyl)-N,2,6-trimethylbenzenamine수율 90.2%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

3.1 ml (4.6 g, 40 mmoles) of methanesulfonyl chloride are added dropwise, at a temperature not exceeding 20° C., to a solution of 7.0 g (36.2 mmoles) of 1-[N-methyl-N-(2,6-dimethylphenyl)-amino]-2-propanol and 5.45 ml (4.0 g, 40 mmoles) of triethyl amine in 50 ml of 1,2-dichloroethane, and the resulting mixture is stirred at room temperature for 3 hours. The mixture is washed then thrice with 30 ml of water, each, dried over anhydrous magnesium sulfate, the solvent is evaporated, and the oily residue is distilled under reduced pressure. 6.9 g (90.2%) of 1-[N-methyl-N-(2,6-dimethylphenyl)-amino]-2-chloro-propane are obtained; b.p.: 116°-118° C./133 Pa.

후처리

  1. washThe mixture is washed
  2. dry with materialeach, dried over anhydrous magnesium sulfate
  3. customthe solvent is evaporated
  4. distillationthe oily residue is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-92a3d90499da4f74afd93da2aa61e499
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04922021

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