Sulfuric Acid → HCID 23054225、化合物

HRID 2250992

反応式

HRID 2250992 の反応式
C(OC(=O)C)(=O)C.[CH:8]1[C:21]2[C:20](=[O:22])[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[O:13][C:12]=2[CH:11]=[CH:10][CH:9]=1.C(O)(=O)C.C(O)(=O)C.[I:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.S(=O)(=O)(O)O.[F:43][B-:44]([F:47])([F:46])[F:45].[K+]>O.C1(C)C=CC=CC=1>[F:43][B-:44]([F:47])([F:46])[F:45].[C:32]1([I+:31][C:9]2[CH:10]=[CH:11][C:12]3[O:13][C:14]4[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=4)[C:20](=[O:22])[C:21]=3[CH:8]=2)[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1

参加物

8

反応物 5

HCID 1118Sulfuric AcidHCID 7020XanthoneHCID 7918Acetic AnhydrideHCID 518872Potassium tetrafluoroborateHCID 12217721Iodo benzene diacetate

生成物 1

HCID 23054225HCID 23054225、化合物収率 47%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

To 80 ml of acetic anhydride were suspended 9.8 g (0.05 mol) of xanthene-9-one and 16.1 g (0.05 mol) of iodobenzene diacetate, and 10 g (0.1 mol) of concentrated sulfuric acid was added dropwise thereto at 0 to 7° C. for 1 hour, followed by gradually warming to room temperature and reacting with stirring for 8 hours. After completion of the reaction, the obtained reaction solution was poured into 200 ml of ice water, and 150 ml of toluene was added thereto to dissolve insoluble substance. The solution was fractionated and 12.6 g (0.1 mol) of potassium tetrafluoroborate was added to the obtained water layer, followed by stirring at room temperature for 2 hours. The precipitated crystal was filtered off and dried at 50° C. under vacuum for 2 hours to obtain 11.4 g of 2-(phenyliodonio)xanthene-9-one tetrafluoroborate as pale orange crystal (yield: 47%).

後処理

  1. additionwas added dropwise
  2. customAfter completion of the reaction
  3. customthe obtained reaction solution
  4. additionwas added
  5. dissolutionto dissolve insoluble substance
  6. stirringby stirring at room temperature for 2 hours
  7. filtrationThe precipitated crystal was filtered off
  8. customdried at 50° C. under vacuum for 2 hours

出典と根拠

ORDレコード
ord-8ca9477e10174bbb8db7a98271ad635c
出典データセット
uspto-grants-2008_01
特許番号
US07318991B2

関連ノート

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