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

HRID 1109830

반응식

HRID 1109830 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]Br.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 24408BromineHCID 64774Pyridine, hydrofluoride (1:1)HCID 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 6344Dichloromethane용매2회

실험 절차

Pyridinium poly(hydrogen fluoride) was added to a solution of 4-chloro-3,6-dihydrophthalic anhydride (6.5 g) in methylene chloride (10.1 g) at room temperature. Bromine (3.1 g) was added. A violent reaction occurs. The solution was allowed to stand for 6 hours and then was poured into a two phase mixture of methylene chloride (30 ml) and solid sodium carbonate. The suspension was stirred for 10 minutes until bubbling stopped. The mixture was filtered and the methylene chloride removed under reduced pressure. The material was purified by a bulb to bulb distillation (140° C. air temperature and 2.8 torr) to give a yellowish solid, (3.74 g).

후처리

  1. customA violent reaction
  2. customuntil bubbling
  3. filtrationThe mixture was filtered
  4. customthe methylene chloride removed under reduced pressure
  5. distillationThe material was purified by a bulb to bulb distillation (140° C. air temperature and 2.8 torr)
  6. customto give a yellowish solid, (3.74 g)

출처 및 근거

ORD 기록
ord-8d4d1e2b6eb74cb0a5fd90834ca6e944
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05322954

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