Hydrochloric Acid → 4,5-Diamino-2',7'-difluoro-3',6'-dihydroxy-spiro[isobenzofuran-1(3H),9'-[9H]-xanthen]-3-one

HRID 1436310노트

반응식

HRID 1436310 반응식
[NH2:1][C:2]1[C:27]([N+:28]([O-])=O)=[CH:26][CH:25]=[C:24]2[C:3]=1[C:4](=[O:31])[O:5][C:6]12[C:19]2[CH:18]=[C:17]([F:20])[C:16]([OH:21])=[CH:15][C:14]=2[O:13][C:12]2[C:7]1=[CH:8][C:9]([F:23])=[C:10]([OH:22])[CH:11]=2.Cl>>[NH2:1][C:2]1[C:27]([NH2:28])=[CH:26][CH:25]=[C:24]2[C:3]=1[C:4](=[O:31])[O:5][C:6]12[C:7]2[CH:8]=[C:9]([F:23])[C:10]([OH:22])=[CH:11][C:12]=2[O:13][C:14]2[C:19]1=[CH:18][C:17]([F:20])=[C:16]([OH:21])[CH:15]=2

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 130077224-Amino-5-nitro-2',7'-difluoro-3',6'-dihydroxy-spiro [isobenzofuran-1(3h),9'-[9h]xanthen]-3-one

생성물 1

HCID 130077234,5-Diamino-2',7'-difluoro-3',6'-dihydroxy-spiro[isobenzofuran-1(3H),9'-[9H]-xanthen]-3-one수율 78.7%

실험 절차

4-Amino-5-nitro-2′,7′-difluoro-3′,6′-dihydroxy-spiro[isobenzofuran-1(3H),9′-[9H]xanthen]-3-one (1.3 g, 3.0 mmol) was added to an aqueous solution of Na2S and NaSH, and the mixture was refluxed for 24 hours. The reaction mixture was cooled, and adjusted to pH 3 with hydrochloric acid, and precipitates were collected by filtration. The obtained product was dried and purified by silica gel chromatography to obtain the title compound (0.94 g, 78%).

후처리

  1. temperaturethe mixture was refluxed for 24 hours
  2. temperatureThe reaction mixture was cooled
  3. customprecipitates
  4. filtrationwere collected by filtration
  5. customThe obtained product was dried
  6. custompurified by silica gel chromatography

출처 및 근거

ORD 기록
ord-52b1851e17874a3ba1a926442a2bd0e5
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618997B2

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