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Hydrochloric Acid → HCID 58380528, 화합물

HRID 1259386
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HRID 1259386 반응식
Cl.Cl[Sn]Cl.O.[F:6][C:7]1[CH:12]=[C:11]([I:13])[CH:10]=[CH:9][C:8]=1[NH:14][C:15]1[C:16]([N+:26]([O-])=O)=[C:17]2[O:25][CH2:24][CH2:23][N:18]2[C:19](=[O:22])[C:20]=1[CH3:21].C(=O)(O)[O-]>C(O)C.C(OC(=O)C)C>[NH2:26][C:16]1[C:15]([NH:14][C:8]2[CH:9]=[CH:10][C:11]([I:13])=[CH:12][C:7]=2[F:6])=[C:20]([CH3:21])[C:19](=[O:22])[N:18]2[CH2:23][CH2:24][O:25][C:17]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 769Bicarbonate IonHCID 43835034Tin dichloride dihydrateHCID 583805937-(2-Fluoro-4-iodo-phenylamino)-6-methyl-8-nitro-2,3-dihydro-oxazolo[3,2-a]pyridin-5-one

생성물 1

HCID 58380528HCID 58380528, 화합물수율 57.5%

시약·촉매·용매 2

HCID 702
Ethanol
용매
HCID 8857Ethyl Acetate용매2회

실험 절차

Concentrated HCl (0.2 mL) and SnCl2.H2O (0.24 g, 1.06 mmol) were added to 7-(2-fluoro-4-iodo-phenylamino)-6-methyl-8-nitro-2,3-dihydro-oxazolo[3,2-a]pyridin-5-one (0.15 g, 0.347 mmol) in ethanol (5 mL). The resulting mixture was heated to reflux for 2 hours. The reaction was monitored by TLC (100% ethylacetate). The reaction mixture was cooled to room temperature, diluted with ethylacetate, basified with saturated bicarbonate solution and filtered through celite. The organic layer was washed with brine solution, dried over Na2SO4 and concentrated to afford 0.08 g of the crude product which was used in the next step without further purification.

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux for 2 hours
  3. filtrationfiltered through celite
  4. washThe organic layer was washed with brine solution
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-591d17101e174c3aa9559ebfca0581dc
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08466289B2

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