Sodium Carbonate → 5Bromo-4-chloro-4-fluoro-3,4,5,6-tetrahydrophthalic anhydride

HRID 1109826

반응식

HRID 1109826 반응식
C1C=CN=CC=1.[FH:7].[Cl:8][C:9]1[CH2:10][C:11]2[C:16](=[O:17])[O:15][C:13](=[O:14])[C:12]=2[CH2:18][CH:19]=1.[Br:20]N1C(=O)CCC1=O.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)Cl>[Br:20][CH:19]1[CH2:18][C:12]2[C:13]([O:15][C:16](=[O:17])[C:11]=2[CH2:10][C:9]1([Cl:8])[F:7])=[O:14]

참가 물질

6

반응물 4

HCID 10340Sodium CarbonateHCID 64774Pyridine, hydrofluoride (1:1)HCID 67184N-bromobutanimideHCID 109869774-Chloro-3,6-dihydrophthalic anhydride

생성물 1

HCID 110980575Bromo-4-chloro-4-fluoro-3,4,5,6-tetrahydrophthalic anhydride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Pyridinium poly(hydrogen fluoride) was added to a solid mixture of 4-chloro-3,6-dihydrophthalic anhydride (0.22 g) and N-bromosuccinimide (0.21 g) at room temperature. The reaction mixture was stirred for 3.25 hours and then carefully poured into a two phase system containing saturated sodium carbonate and methylene chloride. The methylene chloride layer was dried over magnesium sulfate and the solvent removed under reduced pressure. The residue was analyzed by NMR and GC-MS and contained 5-bromo -4-fluoro-3,4,5,6-tetrahydrophthalic anhydride as the major product along with some 4-fluorophthalic anhydride.

후처리

  1. additioncarefully poured into a two phase system
  2. dry with materialThe methylene chloride layer was dried over magnesium sulfate
  3. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-500ce20f28264da08f0ddc01cbb64ed7
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05322954

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