Trifluoroacetic acid → 3-Cyano-4-(3-hydroxymethyl-4-phenoxy-phenylamino)-5-methyl-pyrrolo[1,2-b]pyridazine-6-carboxylic acid ethyl ester

HRID 1796632ノート

反応式

HRID 1796632 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:7]([CH3:39])=[C:8]2[C:13]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([O:21][C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)=[C:17]([CH2:28][O:29]C4CCCCO4)[CH:16]=3)=[C:12]([C:36]#[N:37])[CH:11]=[N:10][N:9]2[CH:38]=1)=[O:5])[CH3:2].C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[C:7]([CH3:39])=[C:8]2[C:13]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([O:21][C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)=[C:17]([CH2:28][OH:29])[CH:16]=3)=[C:12]([C:36]#[N:37])[CH:11]=[N:10][N:9]2[CH:38]=1)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 69327665HCID 69327665、化合物

生成物 1

HCID 696493093-Cyano-4-(3-hydroxymethyl-4-phenoxy-phenylamino)-5-methyl-pyrrolo[1,2-b]pyridazine-6-carboxylic acid ethyl ester収率 43.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 394 (30 mg, 0.057 mmol) in CH2Cl2 (1 ml) was added TFA (300 μl). The mixture was stirred at rt for 30 min, concentrated and purified by silica gel flash column chromatography to give the title compound (11 mg, 44%) (30% EtOAc—Hexanes). LCMS Found: (M+H)+=443.2

後処理

  1. concentrationconcentrated
  2. custompurified by silica gel flash column chromatography

出典と根拠

ORDレコード
ord-6a7f17bf4de14c848a51bc8bbf22276e
出典データセット
uspto-grants-2006_04
特許番号
US07030112B2

反応ノート

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