Hydrochloric Acid → HCID 84716661, 화합물

HRID 2200155노트

반응식

HRID 2200155 반응식
[F:1][C:2]([C:5]1[CH:6]=[C:7]([N:11]=C(C2C=CC=CC=2)C2C=CC=CC=2)[CH:8]=[N:9][CH:10]=1)([F:4])[CH3:3].O.Cl.C1COCC1>CCOC(C)=O>[F:1][C:2]([C:5]1[CH:6]=[C:7]([NH2:11])[CH:8]=[N:9][CH:10]=1)([F:4])[CH3:3]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8028TetrahydrofuranHCID 90020358HCID 90020358, 화합물

생성물 1

HCID 84716661HCID 84716661, 화합물수율 96.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Add 5-(1,1-difluoroethyl)-N-(diphenylmethylene)pyridin-3-amine (296 mg, 0.92 mmol), water (1 mL) and hydrochloric acid (1N, 4 mL) to THF (10 mL), stir at room temperature for 3 hrs. TLC (PE:EtOAc=2:1) shows the reaction is complete. Extract the mixture with ethyl acetate, wash the organic layer with saturated sodium bicarbonate solution and brine sequentially, and dry over anhydrous sodium sulfate. Concentrate under reduced pressure to give the crude product. Purification by flash chromatography (silica gel, EtOAc:PE=1:1) yields the title compound (140 mg, 96.5%). MS: (M+1): 159.2.

후처리

  1. extractionExtract the mixture with ethyl acetate
  2. washwash the organic layer with saturated sodium bicarbonate solution and brine sequentially
  3. dry with materialdry over anhydrous sodium sulfate
  4. concentrationConcentrate under reduced pressure
  5. customto give the crude product
  6. customPurification by flash chromatography (silica gel, EtOAc:PE=1:1)

출처 및 근거

ORD 기록
ord-7c2ef2e7d7584d469c1259c61e875f90
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09359338B2

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