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Hydrochloric Acid → HCID 14722396, 화합물

HRID 1031683
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HRID 1031683 반응식
O1CCOCC1.Cl.C([N:11]([C:16]1[C:32]([O:33][C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)=[CH:31][C:19]2[C:20](=[O:30])[C:21]([C:25]([O:27]CC)=[O:26])=[C:22]([CH3:24])[O:23][C:18]=2[CH:17]=1)[S:12]([CH3:15])(=[O:14])=[O:13])(=O)C>O>[C:25]([C:21]1[C:20](=[O:30])[C:19]2[CH:31]=[C:32]([O:33][C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[C:16]([NH:11][S:12]([CH3:15])(=[O:13])=[O:14])=[CH:17][C:18]=2[O:23][C:22]=1[CH3:24])([OH:27])=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 14722395HCID 14722395, 화합물

생성물 1

HCID 14722396HCID 14722396, 화합물수율 95.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

10 ml of dioxane and 10 ml of 6N hydrochloric acid were added to 500 mg of 7-(N-acetyl-N-methylsulfonylamino)-3-ethoxycarbonyl-2-methyl-6-phenoxy-4H-1-benzopyran-4-one. The mixture was refluxed for 20 minutes. The reaction mixture was cooled to 5°-10° C. 30 ml of water was added thereto. The resulting crystal was collected by filtration and recrystallized from acetic acid to obtain 400 mg (yield: 95.2%) of 3-carboxy-2-methyl-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one having a melting point of 238°-241° C.

후처리

  1. temperatureThe mixture was refluxed for 20 minutes
  2. temperatureThe reaction mixture was cooled to 5°-10° C
  3. filtrationThe resulting crystal was collected by filtration
  4. customrecrystallized from acetic acid

출처 및 근거

ORD 기록
ord-dd287b97859446679d6f0c645939d264
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04954518

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