Sodium Hydroxide → 2-(2-Bromophenylamino)-6-benzoxazolylacetic acid

HRID 1372614ノート

反応式

HRID 1372614 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]1[O:10][C:11]2[CH:17]=[C:16]([CH2:18][C:19]([O:21]CC)=[O:20])[CH:15]=[CH:14][C:12]=2[N:13]=1.[OH-].[Na+]>C1COCC1.CO>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]1[O:10][C:11]2[CH:17]=[C:16]([CH2:18][C:19]([OH:21])=[O:20])[CH:15]=[CH:14][C:12]=2[N:13]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 58779103Ethyl 2-(2-bromophenylamino)-6-benzoxazolylacetate

生成物 1

HCID 587783952-(2-Bromophenylamino)-6-benzoxazolylacetic acid収率 93%

試薬・触媒・溶媒 1

HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

Ethyl 2-(2-bromophenylamino)-6-benzoxazolylacetate (3.82 g, 10.6 mmol) was dissolved in THF-methanol (1:1, 40 ml). To the resulting solution, 1.0M-NaOH (52.0 ml, 52.0 mmol) was added, followed by stirring at room temperature for 1.5 hours. To the residue, which had been obtained by distilling off the solvent under reduced pressure, was acidified with 1.0N-HCl. The crystals thus obtained were collected by filtration under reduced pressure, washed with water and dried overnight under reduced pressure at 60° C., whereby 2-(2-bromophenylamino)-6-benzoxazolylacetic acid (3.40 g, 93%) was obtained as a white crystalline powder.

後処理

  1. customTo the residue, which had been obtained
  2. distillationby distilling off the solvent under reduced pressure
  3. customThe crystals thus obtained
  4. filtrationwere collected by filtration under reduced pressure
  5. washwashed with water
  6. customdried overnight under reduced pressure at 60° C.

出典と根拠

ORDレコード
ord-35dab7dd264f4efa9603ad0f7f6aef0c
出典データセット
uspto-grants-2007_01
特許番号
US07157487B2

反応ノート

読み込み中…