Triacetoxyperiodinane → (Rac)-3-[1-(6-fluoro-1-methyl-1h-indazol-5-yl)-ethyl]-6-(1-methyl-1h-pyrazol-4-yl)-imidazo[1,2-b]pyridazine

HRID 69281ノート

反応式

HRID 69281 の反応式
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8]([CH:11]([C:13]3[CH:14]=[C:15]4[C:19](=[CH:20][C:21]=3[F:22])[N:18]([CH3:23])[N:17]=[CH:16]4)O)=[CH:9][N:10]=2)[N:7]=1.ClC1C=CC2N(C(C(C3C=[C:38]4[C:42](=CC=3F)[N:41]([CH3:46])[N:40]=[CH:39]4)=O)=CN=2)N=1.[CH3:47]C(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>C(Cl)Cl>[F:22][C:21]1[CH:20]=[C:19]2[C:15]([CH:16]=[N:17][N:18]2[CH3:23])=[CH:14][C:13]=1[CH:11]([C:8]1[N:6]2[N:7]=[C:2]([C:38]3[CH:39]=[N:40][N:41]([CH3:46])[CH:42]=3)[CH:3]=[CH:4][C:5]2=[N:10][CH:9]=1)[CH3:47]

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 131731820(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-(6-fluoro-1-methyl-1H-indazol-5-yl)-methanone (rac)-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-(6-fluoro-1-methyl-1H-indazol-5-yl)-methanol

生成物 1

HCID 57917432(Rac)-3-[1-(6-fluoro-1-methyl-1h-indazol-5-yl)-ethyl]-6-(1-methyl-1h-pyrazol-4-yl)-imidazo[1,2-b]pyridazine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-(6-fluoro-1-methyl-1H-indazol-5-yl)-methanone (rac)-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-(6-fluoro-1-methyl-1H-indazol-5-yl)-methanol (Stage 278.4, 4.2 g, 12.66 mmol) was suspended in DCM (250 mL). Dess-Martin periodinane (10.64 g, 38.0 mmol) was added and the mixture was stirred at rt for 1.5 h. The mixture was evaporated to dryness and the residue was taken in 1 M NaOH and sonicated. After 15 min of stirring, it was filtered. The precipitate was dried under vacuum overnight to afford the title compound (tR 1.13 min (conditions 2), MH+=330)

後処理

  1. customThe mixture was evaporated to dryness
  2. customsonicated
  3. stirringAfter 15 min of stirring
  4. filtrationit was filtered
  5. customThe precipitate was dried under vacuum overnight

出典と根拠

ORDレコード
ord-a13de345a6974dab8fedd4a3fc22da45
出典データセット
uspto-grants-2014_09
特許番号
US08822468B2

反応ノート

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