Phosphorus oxychloride → 1H-Indole-3-carboxaldehyde, 1-methyl-2-phenyl-

HRID 1076916

반응식

HRID 1076916 반응식
P(Cl)(Cl)(Cl)=O.[CH3:6][N:7]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:9]=[C:8]1[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[C:22]([O-])(=[O:24])C.[Na+]>CN(C)C=O.O>[CH3:6][N:7]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([CH:22]=[O:24])=[C:8]1[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

6

반응물 3

HCID 24813Phosphorus oxychlorideHCID 770951-Methyl-2-phenylindoleHCID 517045Sodium Acetate

생성물 1

HCID 744681H-Indole-3-carboxaldehyde, 1-methyl-2-phenyl-

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매2회

실험 절차

To 150 ml of dimethylformamide 46 ml of phosphorus oxychloride were added dropwise care being taken that the temperature of the reaction mixture did not rise above 20°C. Subsequently to the obtained mixture 103.5 g of 1-methyl-2-phenylindole dissolved in 200 ml of dimethylformamide were added dropwise. During the addition the reaction mixture was kept at a temperature in the range of 20° to 40°C and thereupon for 1 hour kept between 40° and 45°C. Then the reaction mixture was poured into a solution of 490 g of sodium acetate dissolved in 500 ml of water to which 500 g of ice were added. The precipitated aldehyde was separated by suction, washed with water and methanol.

후처리

  1. customdid not rise above 20°C
  2. additionwere added dropwise
  3. additionDuring the addition the reaction mixture
  4. customwas kept at a temperature in the range of 20° to 40°C
  5. additionwere added
  6. customThe precipitated aldehyde was separated by suction
  7. washwashed with water and methanol

출처 및 근거

ORD 기록
ord-4e8a884b2d294e9c97387df9adea24a5
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03958815

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