Hydrochloric Acid → HCID 86705348、化合物

HRID 1773633ノート

反応式

HRID 1773633 の反応式
[O:1]1CCO[CH:2]1[C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:16]3[N:17]=[C:18]([C:26]4[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=4)[CH:19]=[C:20]([NH:21][CH2:22][CH:23]([CH3:25])[CH3:24])[C:15]3=[N:14][CH:13]=2)=[CH:8][CH:7]=1.Cl.C(=O)([O-])O>CC(C)=O>[CH2:22]([NH:21][C:20]1[C:15]2[N:16]([C:12]([C:9]3[CH:8]=[CH:7][C:6]([CH:2]=[O:1])=[CH:11][CH:10]=3)=[CH:13][N:14]=2)[N:17]=[C:18]([C:26]2[CH:27]=[CH:28][N:29]=[CH:30][CH:31]=2)[CH:19]=1)[CH:23]([CH3:25])[CH3:24]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 769Bicarbonate IonHCID 66695628HCID 66695628、化合物

生成物 1

HCID 86705348HCID 86705348、化合物収率 73%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
23 °C

実験手順

To a solution of 63 mg (152 μmol) 3-[4-(1,3-dioxolan-2-yl)phenyl]-N-isobutyl-6-(pyridin-4-yl)imidazo[1,2-b]pyridazin-8-amine which was prepared according to intermediate example 13b, in 2.8 mL acetone were added 190 μL 4N hydrochloric acid and the mixture was stirred at 23° C. for 2 hours. Saturated hydrogen carbonate solution was added and the mixture was extracted with dichloromethane. The organic phase was dried over sodium sulfate. After filtration and removal of solvent the residue was purified by chromatography to give 41 mg (73%) of the title compound.

後処理

  1. extractionthe mixture was extracted with dichloromethane
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. filtrationAfter filtration and removal of solvent the residue
  4. customwas purified by chromatography

出典と根拠

ORDレコード
ord-15b4ee5810864cefa9b39179ba15eb75
出典データセット
uspto-grants-2016_02
特許番号
US09255100B2

反応ノート

読み込み中…