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Hydrochloric Acid → Methyl 4-(4-fluorobenzyl)-3-methoxycarbonylbenzoate

HRID 2187620
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인쇄 미리보기

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HRID 2187620 반응식
[Br-].[F:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][Zn+])=[CH:5][CH:4]=1.Br[C:12]1[CH:21]=[CH:20][C:15]([C:16]([O:18][CH3:19])=[O:17])=[CH:14][C:13]=1[C:22]([O:24][CH3:25])=[O:23].Cl>O1CCCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd]>[F:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][C:20]2[CH:21]=[CH:12][C:13]([C:22]([O:24][CH3:25])=[O:23])=[CH:14][C:15]=2[C:16]([O:18][CH3:19])=[O:17])=[CH:5][CH:4]=1
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 2824912Dimethyl 4-bromoisophthalateHCID 178505763HCID 178505763, 화합물

생성물 1

HCID 18476032Methyl 4-(4-fluorobenzyl)-3-methoxycarbonylbenzoate

시약·촉매·용매 2

HCID 6505921(1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium촉매
HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

A 2.OM solution of 4-fluorobenzyl zinc bromide in tetrahydrofuran (95 ml, 190 mmol; Negishi, E-i. and King, A. O., J.O.C.1977,42,1821) was added dropwise over 20 minutes to a stirred solution of dimethyl 4-bromoisophthalate (20.0 g, 73.2 mmol) and tris(dibenzylideneacetone)dipalladium(O) (0.67 g,0.73 mmol) in tetrahydrofuran (270 ml) at ambient temperature under an inert atmosphere. During the addition the internal temperature rose to 40° C. The reaction mixture was stirred for 3 hours and then poured into 2M. HCl (1500 ml), cooled in an ice bath and the product extracted into ethyl acetate (3×700 ml). The extracts were washed with water (500 ml), brine (500 ml), dried, and the solvent evaporated under reduced pressure. The residue was taken up in a small quantity of dichloromethane, isohexane added, and the solid which crystallised from the solution, filtered and dried to give methyl 4-(4-fluorobenzyl)-3-methoxycarbonylbenzoate (10.5 g)

후처리

  1. additionDuring the addition the internal temperature
  2. customrose to 40° C
  3. additionpoured into 2M
  4. extractionthe product extracted into ethyl acetate (3×700 ml)
  5. washThe extracts were washed with water (500 ml), brine (500 ml)
  6. customdried
  7. customthe solvent evaporated under reduced pressure
  8. additionadded
  9. customthe solid which crystallised from the solution
  10. filtrationfiltered
  11. customdried

출처 및 근거

ORD 기록
ord-a735db8a0cd6486a8bab4dd3323ed27f
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06410539B1

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