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Sodium Hydroxide → (2-(2-Chloro-6-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetic acid

HRID 1372641
ノート
印刷プレビュー

反応式

HRID 1372641 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][C:10]1[O:11][C:12]2[C:18]([F:19])=[C:17]([CH2:20][C:21]([O:23]C)=[O:22])[CH:16]=[CH:15][C:13]=2[N:14]=1.[OH-].[Na+]>C1COCC1.CO>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][C:10]1[O:11][C:12]2[C:18]([F:19])=[C:17]([CH2:20][C:21]([OH:23])=[O:22])[CH:16]=[CH:15][C:13]=2[N:14]=1
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 58778824Methyl (2-(2-chloro-6-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetate

生成物 1

HCID 17859500(2-(2-Chloro-6-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetic acid収率 93.4%

試薬・触媒・溶媒 1

HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

To a solution of methyl (2-(2-chloro-6-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetate (1.45 g, 4.16 mmol) in THF/methanol (4:1, v/v 100 ml) was added 1N NaOH (40 ml). After stirring at room temperature for 17 hours, the reaction mixture was distilled under reduced pressure to remove the solvent. The residue was acidified with 1N HCl. The crystals thus precipitated were collected by filtration under reduced pressure, washed with water and dried under reduced pressure to give (2-(2-chloro-6-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetic acid (1.30 g, 93%) as a colorless crystalline powder.

後処理

  1. distillationthe reaction mixture was distilled under reduced pressure
  2. customto remove the solvent
  3. customThe crystals thus precipitated
  4. filtrationwere collected by filtration under reduced pressure
  5. washwashed with water
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-ade70f6e237d4bb9aadf133fb61bcfc8
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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