Hydrochloric Acid → 4-(2-(2-Fluoro-5-iodobenzylidene)hydrazinyl)benzoic acid

HRID 13178

반응식

HRID 13178 반응식
[NH:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][CH:4]=1)[NH2:2].[F:12][C:13]1[CH:20]=[CH:19][C:18]([I:21])=[CH:17][C:14]=1[CH:15]=O.C(=O)([O-])[O-].[Cs+].[Cs+].Cl>CN(C=O)C.O>[F:12][C:13]1[CH:20]=[CH:19][C:18]([I:21])=[CH:17][C:14]=1[CH:15]=[N:2][NH:1][C:3]1[CH:4]=[CH:5][C:6]([C:7]([OH:9])=[O:8])=[CH:10][CH:11]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10796Cesium carbonateHCID 120894-Hydrazinobenzoic acidHCID 162170582-Fluoro-5-iodobenzaldehyde

생성물 1

HCID 668129224-(2-(2-Fluoro-5-iodobenzylidene)hydrazinyl)benzoic acid수율 98.1%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

4-hydrazinylbenzoic acid (1.54 g, 10 mmol), 2-fluoro-5-iodobenzaldehyde (2.52 g, 10 mmol) and caesium carbonate (3.27 g, 10 mmol) was stirred in DMF (10 mL) at r.t. for 70 min. Water (40 mL) was then added and the clear solution was acidified with aqueous HCl (1.7 M). The light yellow precipitate that formed was collected by filtration, washed with water and dried in vacuo to give 4-(2-(2-fluoro-5-iodobenzylidene)hydrazinyl)benzoic acid (3.77 g, 98%)

후처리

  1. customThe light yellow precipitate that formed
  2. filtrationwas collected by filtration
  3. washwashed with water
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-56296c7b640b460fa42482a5a0bba46b
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728030B2

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