Diethyl Ether → N-(4-propyl-1,3-dioxolan-2-ylmethyl)-2-methoxy-alpha-chloroacetanilide

HRID 28040노트

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HRID 28040 반응식
[CH2:1]([CH:4]1[CH2:8][O:7][CH:6]([CH2:9][NH:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2OC)[O:5]1)[CH2:2][CH3:3].[CH2:19]([O:21][CH2:22]C)C.[C:24](=[O:27])([O-])[O-].[Na+].[Na+].[Cl:30]CC(Cl)=O>O>[CH2:1]([CH:4]1[CH2:8][O:7][CH:6]([CH2:9][N:10]([C:24](=[O:27])[CH:19]([O:21][CH3:22])[Cl:30])[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[O:5]1)[CH2:2][CH3:3]

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6577Chloroacetyl chlorideHCID 10340Sodium CarbonateHCID 23338370HCID 23338370, 화합물

생성물 1

HCID 23338389N-(4-propyl-1,3-dioxolan-2-ylmethyl)-2-methoxy-alpha-chloroacetanilide

시약·촉매·용매 1

HCID 962Water용매

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온도
5 °C

실험 절차

N-(4-Propyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline (0.25 mole), diethyl ether (30 ml), sodium carbonate (35.5 grams) and water (50 ml) are charged into a glass reaction vessel equipped with stirrer, thermometer and cooling means. The mixture is cooled to about 5° C. and chloroacetyl chloride (0.28 mole) is added dropwise with stirring. After the addition is completed, stirring is continued for 1 hour. After this time the organic phase is separated from the aqueous phase and is filtered. The filtrate is then washed with aqueous sodium carbonate, dried over anhydrous magnesium sulfate and filtered. The filtrate is then stripped of solvent under reduced pressure to yield the desired product N-(4-propyl-1,3-dioxolan-2-ylmethyl)-2-methoxy-α-chloroacetanilide as the residue.

후처리

  1. customequipped with stirrer
  2. temperaturethermometer and cooling means
  3. additionAfter the addition
  4. stirringstirring
  5. customAfter this time the organic phase is separated from the aqueous phase
  6. filtrationis filtered
  7. washThe filtrate is then washed with aqueous sodium carbonate
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered

출처 및 근거

ORD 기록
ord-014ae2fa5ffd4701817a05d6204d0400
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04225335

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