2,4-Dichlorobenzyl chloride → Methyl 2,4-dichloro-alpha-phenylbenzenepropanoate

HRID 1730170

반응식

HRID 1730170 반응식
[C:1]1([CH2:7][C:8]([O:10][CH3:11])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Na+].[Cl:14][C:15]1[CH:20]=[CH:19][C:18]([CH2:21]Cl)=[C:17]([Cl:23])[CH:16]=1>CN(C)C=O.C1C=CC=CC=1>[Cl:23][C:17]1[CH:16]=[C:15]([Cl:14])[CH:20]=[CH:19][C:18]=1[CH2:21][CH:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[C:8]([O:10][CH3:11])=[O:9]

참가 물질

6

반응물 3

HCID 72122,4-Dichlorobenzyl chlorideHCID 7559Methyl phenylacetateHCID 24758Sodium hydride

생성물 1

HCID 21499609Methyl 2,4-dichloro-alpha-phenylbenzenepropanoate

시약·촉매·용매 2

HCID 241Benzene용매2회HCID 6228Dimethylformamide용매2회

실험 절차

A mixture of 30 parts of methyl benzeneacetate, 6.8 parts of sodium hydride dispersion 78%, 135 parts of N,N-dimethylformamide and 180 parts of benzene is stirred for 1 hour at room temperature, while nitrogen gas is introduced. Another 90 parts of benzene is added. Then there is added dropwise, during a 30 minutes-period, a solution of 43.4 parts of 1,3-dichloro-4-(chloromethyl)benzene in 45 parts of N,N-dimethylformamide. Upon completion, stirring is continued for 30 minutes at room temperature. The reaction mixture is poured onto water and the product is extracted twice with 2,2'-oxybispropane. The combined extracts are washed with water, dried, filtered and evaporated. The residue is distilled, yielding 26.5 parts of methyl 2,4-dichloro-α-phenylbenzenepropanoate; bp. 140°-145° C at 0.05 mm. pressure.

후처리

  1. additionis introduced
  2. additionThen there is added dropwise, during a 30 minutes-period
  3. stirringUpon completion, stirring
  4. waitis continued for 30 minutes at room temperature
  5. additionThe reaction mixture is poured onto water
  6. extractionthe product is extracted twice with 2,2'-oxybispropane
  7. washThe combined extracts are washed with water
  8. customdried
  9. filtrationfiltered
  10. customevaporated
  11. distillationThe residue is distilled

출처 및 근거

ORD 기록
ord-ecd323c52d5446afb5cfdd0746570e8f
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03991201

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