Sodium Hydroxide → HCID 89501036、化合物

HRID 1525359ノート

反応式

HRID 1525359 の反応式
[Cl:1][C:2]1[C:3]([F:19])=[CH:4][C:5]([N:14]2[CH:18]=[N:17][N:16]=[N:15]2)=[C:6](/[CH:8]=[CH:9]/[C:10]([O:12]C)=[O:11])[CH:7]=1.[OH-].[Na+]>CO.C1COCC1>[Cl:1][C:2]1[C:3]([F:19])=[CH:4][C:5]([N:14]2[CH:18]=[N:17][N:16]=[N:15]2)=[C:6](/[CH:8]=[CH:9]/[C:10]([OH:12])=[O:11])[CH:7]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 89501016HCID 89501016、化合物

生成物 1

HCID 89501036HCID 89501036、化合物収率 42.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To Intermediate 5C (5 g, 17.7 mmol) in MeOH (50 mL) and THF (25 mL) was added 10% NaOH solution (25 mL). After 2 h, the reaction was concentrated and the residue was diluted with H2O. The pH was adjusted to 2 to 3 with 1.5 N HCl and the resultant solid was filtered and washed with petroleum ether to afford 2 g of Intermediate 5. MS (ESI) m/z: 269.0 (M+H)+.

後処理

  1. concentrationthe reaction was concentrated
  2. additionthe residue was diluted with H2O
  3. filtrationthe resultant solid was filtered
  4. washwashed with petroleum ether

出典と根拠

ORDレコード
ord-f113eadd17b046029e4aaa97ee2043d0
出典データセット
uspto-grants-2015_07
特許番号
US09079929B2

反応ノート

読み込み中…