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Sodium Hydroxide → HCID 44606816、化合物

HRID 1372574
ノート
印刷プレビュー

反応式

HRID 1372574 の反応式
[F:1][C:2]1[C:10]2[O:9][C:8]([NH:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])=[N:7][C:6]=2[CH:5]=[CH:4][C:3]=1[CH2:19][C:20]([O:22]C)=[O:21].[OH-].[Na+]>C1COCC1>[F:1][C:2]1[C:10]2[O:9][C:8]([NH:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])=[N:7][C:6]=2[CH:5]=[CH:4][C:3]=1[CH2:19][C:20]([OH:22])=[O:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 58778451Methyl 7-fluoro-2-(2-methylphenylamino)-6-benzoxazolylacetate

生成物 1

HCID 44606816HCID 44606816、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 7-fluoro-2-(2-methylphenylamino)-6-benzoxazolylacetate (1.31 g, 4.17 mmol) was dissolved in THF (30 ml), followed by the addition of 0.25N NaOH (30 ml). The resulting mixture was stirred at room temperature for 20 hours. The reaction mixture was distilled under reduced pressure to remove the solvent. The residue was acidified with 1N HCl, followed by extraction with a chloroform/methanol (10/1) mixture. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and distilled under reduced pressure to remove the solvent, whereby the title compound (1.08 g, 86%) was obtained as a pale brown solid.

後処理

  1. distillationThe reaction mixture was distilled under reduced pressure
  2. customto remove the solvent
  3. extractionfollowed by extraction with a chloroform/methanol (10/1) mixture
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationdistilled under reduced pressure
  7. customto remove the solvent, whereby the title compound (1.08 g, 86%)
  8. customwas obtained as a pale brown solid

出典と根拠

ORDレコード
ord-b0cd3d13784d44589152c1dad6b10ce4
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07157487B2

反応ノート

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