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

HRID 1109826

反応式

HRID 1109826 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]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]

参加物

6

反応物 4

HCID 10340Sodium CarbonateHCID 64774Pyridine, hydrofluoride (1:1)HCID 67184N-bromobutanimideHCID 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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-500ce20f28264da08f0ddc01cbb64ed7
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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