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Sodium Hydroxide → HCID 178433944、化合物

HRID 985440
ノート
印刷プレビュー

反応式

HRID 985440 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[N:13]2[N:14]=[C:15]([O:17]S(C3C=CC(C)=CC=3)(=O)=O)[CH:16]=[C:12]2[C:11]([CH3:28])=[N:10][N:9]=1.[OH-].[Na+]>O1CCOCC1.O>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[N:13]2[N:14]=[C:15]([OH:17])[CH:16]=[C:12]2[C:11]([CH3:28])=[N:10][N:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 87418381Toluene-4-sulfonic acid 7-(2-fluorophenyl)-4-methylpyrazolo[1,5-d][1,2,4]triazin-2-yl ester

生成物 1

HCID 178433944HCID 178433944、化合物収率 95.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a stirred solution of toluene-4-sulfonic acid 7-(2-fluorophenyl)-4-methylpyrazolo[1,5-d][1,2,4]triazin-2-yl ester (3.39 g, 8.51 mmol) in 1,4-dioxane (150 ml) and water (30 ml) was added 4 N aqueous NaOH (10.64 ml, 42.6 mmol) and the mixture was stirred at room temperature for 4 h. The mixture was concentrated in vacuo to about 30 ml, and the aqueous residue was diluted with water (150 ml) and washed with ethyl acetate (50 ml). The remaining aqueous layer was acidified to pH 5 with 5 N aqueous HCl (4 ml) and the resulting precipitate was collected by filtration, washed with water and dried at 60° C. under vacuum to leave 1.98 g (95%) of the title compound as a cream solid: 1H NMR (360 MHz, DMSO-d6) δ 2.68 (3H, s), 6.38 (1H, s), 7.41-7.47 (2H, m), 7.66-7.77 (2H, m); MS (ES+) m/e 245 [M+H]+.

後処理

  1. concentrationThe mixture was concentrated in vacuo to about 30 ml
  2. additionthe aqueous residue was diluted with water (150 ml)
  3. washwashed with ethyl acetate (50 ml)
  4. filtrationthe resulting precipitate was collected by filtration
  5. washwashed with water
  6. customdried at 60° C. under vacuum

出典と根拠

ORDレコード
ord-9a2fc35adb554ba8ab25bcde0e50afa2
出典データセット
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06872720B2

反応ノート

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