Hydrochloric Acid → 2-(4-{4-[(2-Amino-6-chloropyrimidin-4-yl)amino]-2-fluorophenoxy}-1H-pyrrolo[2,3-b]pyridin-3-yl)ethanol

HRID 2192188ノート

反応式

HRID 2192188 の反応式
[NH2:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]3[NH:13][CH:14]=[C:15]([CH2:16][CH2:17][OH:18])[C:8]=23)=[C:4]([F:21])[CH:3]=1.[Cl:22][C:23]1[CH:28]=[C:27](Cl)[N:26]=[C:25]([NH2:30])[N:24]=1.Cl.[OH-].[Na+]>O>[NH2:30][C:25]1[N:26]=[C:27]([NH:1][C:2]2[CH:20]=[CH:19][C:5]([O:6][C:7]3[CH:12]=[CH:11][N:10]=[C:9]4[NH:13][CH:14]=[C:15]([CH2:16][CH2:17][OH:18])[C:8]=34)=[C:4]([F:21])[CH:3]=2)[CH:28]=[C:23]([Cl:22])[N:24]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 655222-Amino-4,6-dichloropyrimidineHCID 210815442-[4-(4-Amino-2-fluorophenoxy)-1H-pyrrolo[2,3-b]pyridin-3-yl]ethanol

生成物 1

HCID 116113682-(4-{4-[(2-Amino-6-chloropyrimidin-4-yl)amino]-2-fluorophenoxy}-1H-pyrrolo[2,3-b]pyridin-3-yl)ethanol

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

56 mg (0.17 mmol) of 2-[4-(4-amino-2-fluorophenoxy)-1H-pyrrolo[2,3-b]pyridin-3-yl]ethanol and 30 mg (0.18 mmol) of 4,6-dichloropyrimidine-2-amine are suspended in 5 ml of water. 25 μl of 37% strength hydrochloric acid are added, and the mixture is heated at reflux overnight. Using 1N aqueous sodium hydroxide solution, the pH is then adjusted to 10, resulting in the precipitation of crystals. The mixture is concentrated and filtered through silica gel. The product is purified by preparative HPLC.

後処理

  1. temperaturethe mixture is heated
  2. temperatureat reflux overnight
  3. customresulting in the precipitation of crystals
  4. concentrationThe mixture is concentrated
  5. filtrationfiltered through silica gel
  6. customThe product is purified by preparative HPLC

出典と根拠

ORDレコード
ord-0fd108df6e8a457aabf112fdd3166f23
出典データセット
uspto-grants-2012_12
特許番号
US08329716B2

反応ノート

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