Trifluoroacetic anhydride → 2-Cyclopropyl-6-iodo-3-methylimidazo[1,2-a]pyridine

HRID 60382노트

반응식

HRID 60382 반응식
[CH:1]1([C:4](=O)[CH:5]([N:7]2[CH:12]=[C:11]([I:13])[CH:10]=[CH:9][C:8]2=[N:14]S(C2C=CC(C)=CC=2)(=O)=O)[CH3:6])[CH2:3][CH2:2]1.FC(F)(F)C(OC(=O)C(F)(F)F)=O>C1COCC1>[CH:1]1([C:4]2[N:14]=[C:8]3[CH:9]=[CH:10][C:11]([I:13])=[CH:12][N:7]3[C:5]=2[CH3:6])[CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 131735781N-(1-(1-Cyclopropyl-1-oxopropan-2-yl)-5-iodopyridin-2(1H)-ylidene)-4-methylbenzenesulfonamide

생성물 1

HCID 896903982-Cyclopropyl-6-iodo-3-methylimidazo[1,2-a]pyridine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of N-(1-(1-cyclopropyl-1-oxopropan-2-yl)-5-iodopyridin-2(1H)-ylidene)-4-methylbenzenesulfonamide (30.5 g) in THF (300 mL) was added trifluoroacetic anhydride (18.3 mL) dropwise, and the mixture was stirred for 3 hr. The resulting precipitate was collected by filtration, and washed with diethyl ether to give a salt of the title compound as a white solid. The obtained solid was dissolved in 1 N sodium hydroxide, and the solution was extracted with ethyl acetate/THF. Then the organic layer was washed with brine, dried over sodium sulfate and concentrated in vacuo. The obtained solid was washed with diisopropyl ether to give the title compound (17.7 g) as a yellow solid.

후처리

  1. filtrationThe resulting precipitate was collected by filtration
  2. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-6db0c35485e640179f32a44cfd03d72d
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440987B2

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