Hydrochloric Acid → N-[5-Methyl-2-(2-methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-phenyl]-methanesulfonamide

HRID 1262352노트

반응식

HRID 1262352 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:9]2[N:17]3[C:12]([CH:13]=[N:14][C:15]([S:18][CH3:19])=[N:16]3)=[CH:11][CH:10]=2)=[C:6]([NH2:8])[CH:7]=1.N1C=CC=CC=1.[CH3:26][S:27](Cl)(=[O:29])=[O:28].Cl>>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:9]2[N:17]3[C:12]([CH:13]=[N:14][C:15]([S:18][CH3:19])=[N:16]3)=[CH:11][CH:10]=2)=[C:6]([NH:8][S:27]([CH3:26])(=[O:29])=[O:28])[CH:7]=1

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 667127275-Methyl-2-(2-methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-phenylamine

생성물 1

HCID 66712100N-[5-Methyl-2-(2-methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-phenyl]-methanesulfonamide

실험 절차

To a mixture of 5-Methyl-2-(2-methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-phenylamine (480 mg, 1.8 mmol) in dry pyridine (4 mL, 50 mmol) was added at 0° C. methanesulfonyl chloride (160 uL, 2.1 mmol). The mixture was stirred for 2 h and was thrown to 3N HCl. The mixture was extracted from EtOAc. Combined organic was washed with brine and was dried. After solvent evaporation, the product, N-[5-Methyl-2-(2-methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-phenyl]-methanesulfonamide, was obtained as a yellow solid (591 mg, 96%). The solid was used directly for the next step.

후처리

  1. extractionThe mixture was extracted from EtOAc
  2. washCombined organic was washed with brine
  3. customwas dried
  4. customAfter solvent evaporation

출처 및 근거

ORD 기록
ord-6fec2b9e34bf4bd0a412f0a4ff834060
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08471005B2

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