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Hydrochloric Acid → 6-(4-Fluorophenyl)-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)phenyl]-pyrimidine-2,4-diamine

HRID 16445
ノート
印刷プレビュー

反応式

HRID 16445 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]2[NH:16][CH:17]=[CH:18][C:11]=12)[NH2:5].Cl[C:20]1[CH:25]=[C:24]([C:26]2[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=2)[N:23]=[C:22]([NH2:33])[N:21]=1.Cl.C(=O)([O-])[O-].[Na+].[Na+]>O.CN(C)C=O.C(OCC)(=O)C>[F:32][C:29]1[CH:28]=[CH:27][C:26]([C:24]2[N:23]=[C:22]([NH2:33])[N:21]=[C:20]([NH:5][C:4]3[CH:6]=[CH:7][C:8]([O:9][C:10]4[CH:15]=[CH:14][N:13]=[C:12]5[NH:16][CH:17]=[CH:18][C:11]=45)=[C:2]([F:1])[CH:3]=3)[CH:25]=2)=[CH:31][CH:30]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 112183534-Chloro-6-(4-fluorophenyl)pyrimidin-2-amineHCID 160379654-((1H-Pyrrolo[2,3-B]pyridin-4-YL)oxy)-3-fluoroaniline

生成物 1

HCID 587332456-(4-Fluorophenyl)-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)phenyl]-pyrimidine-2,4-diamine

試薬・触媒・溶媒 3

HCID 6228
Dimethylformamide
触媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

36 mg (0.15 mmol) of 3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)aniline (from example XIX) and 38.5 mg (0.15 mmol) of 4-chloro-6-(4-fluorophenyl)pyrimidine-2-amine (from example LIX) are suspended in 1.5 ml of water, and 0.1 ml of 2 molar hydrochloric acid is added. The mixture is heated under reflux overnight. Ethyl acetate and a few drops of dimethylformamide are then added. The mixture is made alkaline using saturated sodium carbonate solution, the organic phase is separated off and the solvent is removed under reduced pressure. The product is purified by preparative HPLC.

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux overnight
  3. customthe organic phase is separated off
  4. customthe solvent is removed under reduced pressure
  5. customThe product is purified by preparative HPLC

出典と根拠

ORDレコード
ord-6a13486060884f89b5d33e9e22cce4c7
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07737153B2

反応ノート

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