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Ammonia → HCID 23153317、化合物

HRID 492861
ノート
印刷プレビュー

反応式

HRID 492861 の反応式
[NH2:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][C:7]2[CH:12]=[C:11](Cl)[N:10]=[CH:9][N:8]=2)=[CH:4][C:3]=1[F:16].[NH3:17]>O1CCCC1.CO>[NH2:17][C:11]1[CH:12]=[C:7]([O:6][C:5]2[CH:14]=[CH:15][C:2]([NH2:1])=[C:3]([F:16])[CH:4]=2)[N:8]=[CH:9][N:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 222AmmoniaHCID 231530834-[(6-Chloropyrimidin-4-yl)oxy]-2-fluoroaniline

生成物 1

HCID 23153317HCID 23153317、化合物収率 35%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

After dissolving 4-(4-amino-3-fluorophenoxy)-6-chloropyrimidine (2.25 g) in tetrahydrofuran (25 ml) and a 7N ammonia solution in methanol (50 ml), the mixture was heated in a sealed tube for 3 days at 130° C. The reaction mixture was cooled to room temperature and then partitioned between ethyl acetate and 1N aqueous sodium hydroxide. The separated organic layer was washed with brine. The aqueous layer was then re-extracted with ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography (eluent; heptane:ethyl acetate=1:3, then ethyl acetate) to provide the title compound (0.73 g, 35%) as a purple solid.

後処理

  1. custompartitioned between ethyl acetate and 1N aqueous sodium hydroxide
  2. washThe separated organic layer was washed with brine
  3. extractionThe aqueous layer was then re-extracted with ethyl acetate
  4. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off
  6. customthe residue was purified by silica gel column chromatography (eluent

出典と根拠

ORDレコード
ord-0aa99af7eb84487898b445a63438a081
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531532B2

反応ノート

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