Hydrochloric Acid → HCID 84716661、化合物

HRID 2200155ノート

反応式

HRID 2200155 の反応式
[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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8028TetrahydrofuranHCID 90020358HCID 90020358、化合物

生成物 1

HCID 84716661HCID 84716661、化合物収率 96.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-7c2ef2e7d7584d469c1259c61e875f90
出典データセット
uspto-grants-2016_06
特許番号
US09359338B2

反応ノート

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