Sulfuric Acid → HCID 23054225, 화합물

HRID 2250992

반응식

HRID 2250992 반응식
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

참가 물질

8

반응물 5

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

생성물 1

HCID 23054225HCID 23054225, 화합물수율 47%

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-8ca9477e10174bbb8db7a98271ad635c
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07318991B2

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