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

HRID 1109830

反応式

HRID 1109830 の反応式
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]

参加物

6

反応物 4

HCID 10340Sodium CarbonateHCID 24408BromineHCID 64774Pyridine, hydrofluoride (1:1)HCID 109869774-Chloro-3,6-dihydrophthalic anhydride

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-8d4d1e2b6eb74cb0a5fd90834ca6e944
出典データセット
uspto-grants-1994_06
特許番号
US05322954

関連ノート

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