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Sodium Bicarbonate → HCID 58155241, 화합물

HRID 1929475
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HRID 1929475 반응식
C(=[N:14][C:15]1[CH:16]=[CH:17][C:18]([F:31])=[C:19]([C:21]2([CH:28]3[CH2:30][CH2:29]3)[NH:26][C:25](=[S:27])[CH2:24][O:23][CH2:22]2)[CH:20]=1)(C1C=CC=CC=1)C1C=CC=CC=1.C(=O)([O-])O.[Na+]>O1CCOCC1.Cl>[NH2:14][C:15]1[CH:16]=[CH:17][C:18]([F:31])=[C:19]([C:21]2([CH:28]3[CH2:29][CH2:30]3)[NH:26][C:25](=[S:27])[CH2:24][O:23][CH2:22]2)[CH:20]=1
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참가 물질

5

반응물 2

HCID 516892Sodium BicarbonateHCID 58155199HCID 58155199, 화합물

생성물 1

HCID 58155241HCID 58155241, 화합물

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 312751,4-Dioxane용매

실험 절차

A solution of (RS)-5-[5-(benzhydrylidene-amino)-2-fluoro-phenyl]-5-cyclopropyl-morpholine-3-thione (1.42 g, 3.3 mmol) in dioxane (15 ml) and 1 M HCl (5 ml) was stirred at room temperature for 30 minutes. The reaction mixture was poured on a saturated solution of sodium hydrogen-carbonate and extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and evaporated at reduced pressure. The residue was purified by chromatography on silica gel using a 3:1-mixture of dichloromethane and ethyl acetate as the eluent. CH2Cl2/EtOAc 3:1. The (RS)-5-(5-amino-2-fluoro-phenyl)-5-cyclopropyl-morpholine-3-thione was obtained as a white solid (0.810 g, 92% of theory). Mass (calculated) C13H15FN2OS [266.338]; (found) [M+H]+=267.

후처리

  1. extractionextracted twice with ethyl acetate
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated at reduced pressure
  6. customThe residue was purified by chromatography on silica gel using a 3

출처 및 근거

ORD 기록
ord-95f0001178d5437c83dc82f98718dd73
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08188079B2

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