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Hydrochloric Acid → HCID 86640673、化合物

HRID 1645231
ノート
印刷プレビュー

反応式

HRID 1645231 の反応式
[F:1][C:2]([F:6])([F:5])[CH2:3][OH:4].[H-].[Na+].Br[CH2:10][C:11]1[CH:16]=[C:15]([C:17]2[C:22]([Cl:23])=[CH:21][C:20]([C:24]([F:27])([F:26])[F:25])=[CH:19][N:18]=2)[N:14]2[N:28]=[CH:29][N:30]=[C:13]2[N:12]=1.Cl>O1CCCC1>[Cl:23][C:22]1[C:17]([C:15]2[N:14]3[N:28]=[CH:29][N:30]=[C:13]3[N:12]=[C:11]([CH2:10][O:4][CH2:3][C:2]([F:6])([F:5])[F:1])[CH:16]=2)=[N:18][CH:19]=[C:20]([C:24]([F:26])([F:25])[F:27])[CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 64092,2,2-TrifluoroethanolHCID 24758Sodium hydrideHCID 66775659HCID 66775659、化合物

生成物 1

HCID 86640673HCID 86640673、化合物収率 30.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

230 mg of 2,2,2-trifluoroethanol was added to a tetrahydrofuran (dehydrated) 8 mL solution of 33 mg of 60% sodium hydride, followed by stirring for 5 minutes, and 300 mg of 5-bromomethyl-7-(3-chloro-5-(trifluoromethyl)pyridin-2-yl)-[1,2,4]triazolo[1,5-a]pyrimidine was added at room temperature, followed by stirring for 5 minutes. After completion of the reaction, 1N hydrochloric acid was added to make it acidic, followed by extraction with ethyl acetate, the organic layer was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1) to obtain 97 mg of the desired product.

後処理

  1. stirringby stirring for 5 minutes
  2. additionwas added
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1)

出典と根拠

ORDレコード
ord-3a39aaf838ea424a88e46147c48e0f6a
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08124760B2

反応ノート

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