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

HRID 1262352ノート

反応式

HRID 1262352 の反応式
[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

参加物

5

反応物 4

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

生成物 1

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

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-6fec2b9e34bf4bd0a412f0a4ff834060
出典データセット
uspto-grants-2013_06
特許番号
US08471005B2

反応ノート

読み込み中…