4-Fluorobenzohydrazide → HCID 178465640, 화합물

HRID 418268

반응식

HRID 418268 반응식
[OH:1][C@H:2]([C:9]1[N:10]=[C:11]([C:14](=O)[CH3:15])[NH:12][CH:13]=1)[C@H:3]([OH:8])[C@H:4]([OH:7])[CH2:5][OH:6].[F:17][C:18]1[CH:27]=[CH:26][C:21]([C:22]([NH:24][NH2:25])=[O:23])=[CH:20][CH:19]=1>C(O)C.O.Cl>[F:17][C:18]1[CH:27]=[CH:26][C:21]([C:22]([NH:24]/[N:25]=[C:14](/[C:11]2[NH:12][CH:13]=[C:9]([C@@H:2]([OH:1])[C@H:3]([OH:8])[C@H:4]([OH:7])[CH2:5][OH:6])[N:10]=2)\[CH3:15])=[O:23])=[CH:20][CH:19]=1

참가 물질

6

반응물 2

HCID 99724-FluorobenzohydrazideHCID 178467425HCID 178467425, 화합물

생성물 1

HCID 178465640HCID 178465640, 화합물

시약·촉매·용매 3

HCID 313Hydrochloric Acid촉매HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
55 °C

실험 절차

1-[4-((1R,2S,3R)-1,2,3,4-Tetrahydroxy-butyl)-1H-imidazol-2-yl]-ethanone (172 mg, 0.74 mmol) was suspended in ethanol (4 ml) and water (1 ml). 4-fluorobenzoic acid hydrazide (131 mg, 0.85 mmol, 1.1 eq.) and hydrochloric acid (one drop, 12 N) were added, and the suspension was stirred at 55° C. for 48 hours. LCMS analysis indicated the formation of the product and the absence of starting material. The reaction mixture was cooled to room temperature, and partially concentrated in vacuo. The resulting white precipitate was collected and washed with ethanol to yield the product, as one apparent isomer, as a white solid: 97 mg (35%).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationpartially concentrated in vacuo
  3. customThe resulting white precipitate was collected
  4. washwashed with ethanol
  5. customto yield the product

출처 및 근거

ORD 기록
ord-af6617beafb54e54ae6c173fd60f5885
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093267B2

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