2,6-Dichlorobenzaldehyde → (3-Chloro-1,1-dimethylpropyl)-(2,6-dichlorobenzylidene)-amine

HRID 1350912

반응식

HRID 1350912 반응식
Cl.[Cl:2][CH2:3][CH2:4][C:5]([NH2:8])([CH3:7])[CH3:6].[OH-].[Na+].[Cl:11][C:12]1[CH:19]=[CH:18][CH:17]=[C:16]([Cl:20])[C:13]=1[CH:14]=O>C(Cl)Cl>[Cl:2][CH2:3][CH2:4][C:5]([N:8]=[CH:14][C:13]1[C:12]([Cl:11])=[CH:19][CH:18]=[CH:17][C:16]=1[Cl:20])([CH3:7])[CH3:6]

참가 물질

5

반응물 3

HCID 67372,6-DichlorobenzaldehydeHCID 14798Sodium HydroxideHCID 21094547686746-12-3

생성물 1

HCID 21094546(3-Chloro-1,1-dimethylpropyl)-(2,6-dichlorobenzylidene)-amine수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

13.3 g (84.0 mmol) of 3-chloro-1,1-dimethyl propylamine-hydrochloride were added to 84.0 mL sodium hydroxide solution (1 M) at 0° C. with vigorous stirring. The reaction mixture was stirred for 30 min at 0° C. and then combined with 50 mL methylene chloride. The phases were separated and the aqueous phase was twice extracted with 35 mL methylene chloride. The combined organic phases were dried over magnesium sulphate and at ambient temperature combined with 14.2 g (81.0 mmol) of 2,6-dichlorobenzaldehyde with stirring. The reaction mixture was stirred for 18 h at ambient temperature, dried again with magnesium sulphate and the solvent was removed. 22.3 g (80.0 mmol, 99%) (3-chloro-1,1-dimethylpropyl)-(2,6-dichlorobenzylidene)-amine were obtained as a yellowish oil.

후처리

  1. customThe phases were separated
  2. extractionthe aqueous phase was twice extracted with 35 mL methylene chloride
  3. dry with materialThe combined organic phases were dried over magnesium sulphate and at ambient temperature
  4. stirringwith stirring
  5. stirringThe reaction mixture was stirred for 18 h at ambient temperature
  6. dry with materialdried again with magnesium sulphate
  7. customthe solvent was removed

출처 및 근거

ORD 기록
ord-97b6c5badb5e4b48ab2cce294e41862e
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07214698B2

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