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Sodium Hydroxide → HCID 178433944, 화합물

HRID 985440
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HRID 985440 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

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

생성물 1

HCID 178433944HCID 178433944, 화합물수율 95.3%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-9a2fc35adb554ba8ab25bcde0e50afa2
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06872720B2

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