Sodium Hydroxide → 9-Trifluoromethoxy-6H-1,3,3a,6-tetraaza-benzo[e]azulen-5-one

HRID 2066405노트

반응식

HRID 2066405 반응식
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][C:13]([F:16])([F:15])[F:14])=[CH:8][C:7]=1[C:17]1[NH:18][N:19]=[CH:20][N:21]=1)=[O:4].[OH-].[Na+].[Cl-].[NH4+]>O1CCOCC1>[F:14][C:13]([F:16])([F:15])[O:12][C:9]1[CH:10]=[CH:11][C:6]2[NH:5][C:3](=[O:4])[CH2:2][N:18]3[C:17](=[N:21][CH:20]=[N:19]3)[C:7]=2[CH:8]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 686936732-Chloro-N-[2-(2H-[1,2,4]triazol-3-yl)-4-trifluoromethoxy-phenyl]-acetamide

생성물 1

HCID 1363351829-Trifluoromethoxy-6H-1,3,3a,6-tetraaza-benzo[e]azulen-5-one수율 24.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of 2-chloro-N-[2-(2H-[1,2,4]triazol-3-yl)-4-trifluoromethoxy-phenyl]-acetamide (3.15 g, 9.82 mmol) in dioxane (100 mL) was added aqueous sodium hydroxide (32%, 2.18 mL, 23.6 mmol) and the reaction mixture was stirred for 19 h at ambient temperature. It was poured onto aqueous ammonium chloride (1M, 50 mL) and the organic solvent was removed by destillation. The resulting suspension was filtered and the solid was washed with ice-cold water (50 mL). Drying in vacuo afforded the title compound (682 mg, 24%) as a light yellow solid. MS: m/e=285.0 [M+H]+.

후처리

  1. customthe organic solvent was removed by destillation
  2. filtrationThe resulting suspension was filtered
  3. washthe solid was washed with ice-cold water (50 mL)
  4. customDrying in vacuo

출처 및 근거

ORD 기록
ord-b80b6a55267c4d128bd4fbc4e17a78b7
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293730B2

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