Potassium Iodide → 2-(Ethylamino)-4,5-dimethylthiophene-3-carbonitrile

HRID 711626노트

반응식

HRID 711626 반응식
[CH2:1]([NH:8][C:9]1[S:10][C:11]([CH3:17])=[C:12]([CH3:16])[C:13]=1[C:14]#[N:15])[C:2]1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].C(I)C>C(#N)C.C(OCC)(=O)C>[CH2:1]([NH:8][C:9]1[S:10][C:11]([CH3:17])=[C:12]([CH3:16])[C:13]=1[C:14]#[N:15])[CH3:2]

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 3194512-(Benzylamino)-4,5-dimethylthiophene-3-carbonitrile

생성물 1

HCID 574569162-(Ethylamino)-4,5-dimethylthiophene-3-carbonitrile

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 2-(benzylamino)-4,5-dimethylthiophene-3-carbonitrile (302 mg, 2.0 mmol), potassium carbonate (276 mg, 2.0 mmol), and a catalytic amount of potassium iodide in acetonitrile (1 mL) in a 20 mL microwave vial was added ethyl iodide (310 mg, 2.0 mmol). The reaction vial was placed in a microwave reactor for 15 minutes at 165° C. The reaction mixture was dissolved in ethyl acetate and washed with water and brine. The ethyl acetate portion was dried over sodium sulfate and solvent was evaporated under reduced pressure, and the product was purified by prep HPLC using acetonitrile/water as solvent. MS 181 (MH+).

후처리

  1. customThe reaction
  2. washwashed with water and brine
  3. dry with materialThe ethyl acetate portion was dried over sodium sulfate and solvent
  4. customwas evaporated under reduced pressure
  5. customthe product was purified by prep HPLC

출처 및 근거

ORD 기록
ord-69a0d9ea05ba4acfaaee5b555d7a9fe9
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181276B2

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