Chloroform → HCID 86667593, 화합물

HRID 85304노트

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HRID 85304 반응식
P(Cl)(Cl)(Cl)=O.[CH2:6]([NH:10][C:11]1[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[C:13]([O:19][CH3:20])[CH:12]=1)[CH2:7][CH2:8][CH3:9].C(Cl)(Cl)Cl.CN(C)[CH:27]=[O:28]>>[CH2:6]([N:10]([CH2:6][CH2:7][CH2:8][CH3:9])[C:11]1[CH:16]=[C:15]([O:17][CH3:18])[C:14]([CH:27]=[O:28])=[C:13]([O:19][CH3:20])[CH:12]=1)[CH2:7][CH2:8][CH3:9]

참가 물질

5

반응물 4

HCID 6212ChloroformHCID 6228Dimethylformamide2회HCID 24813Phosphorus oxychlorideHCID 137939884-Butylamino-2,6-dimethoxybenzene

생성물 1

HCID 86667593HCID 86667593, 화합물수율 80%

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온도
7.5 °C

실험 절차

In a stream of argon, to 30 ml of N,N-dimethylformamide was added 16.0 g (104 mmol) of phosphorus oxychloride under cooling at 5 to 10° C. and stirring. After the mixture was well-stirred, 23.5 g (80.1 mmol) of 4-butylamino-2,6-dimethoxybenzene dissolved in 10 ml of N,N-dimethylformamide was added dropwise. The mixture was reacted with stirring for 1.5 hours. After the mixture was poured into 70 ml of ice water, extraction with 200 ml of chloroform, washing with a saturated saline solution, drying over anhydrous magnesium sulfate, and concentration were performed. The residue was purified by silica gel chromatography to give 18.8 g (yield: 80%) of 4-dibutylamino-2,6-dimethoxybenzaldehyde as a dark purple crystal (mp: 55-56° C.)

후처리

  1. stirringAfter the mixture was well-stirred
  2. additionwas added dropwise
  3. customThe mixture was reacted
  4. stirringwith stirring for 1.5 hours
  5. washwashing with a saturated saline solution
  6. dry with materialdrying over anhydrous magnesium sulfate, and concentration
  7. customThe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-46197a9033de47c596ab244156fbcaf9
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846955B2

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