Amitrole → HCID 178515486, 화합물

HRID 923342

반응식

HRID 923342 반응식
[N:1]1[NH:2][C:3]([NH2:6])=[N:4][CH:5]=1.[O:7]1[CH2:12][CH2:11][O:10][C:9]2[CH:13]=[C:14]([C:17](=O)[CH2:18][C:19](OCC)=[O:20])[CH:15]=[CH:16][C:8]1=2>C(O)(=O)C>[O:7]1[CH2:12][CH2:11][O:10][C:9]2[CH:13]=[C:14]([C:17]3[NH:6][C:3]4[N:2]([N:1]=[CH:5][N:4]=4)[C:19](=[O:20])[CH:18]=3)[CH:15]=[CH:16][C:8]1=2

참가 물질

4

반응물 2

HCID 1639AmitroleHCID 15315318Ethyl 2,3-dihydro-β-oxo-1,4-benzodioxin-6-propanoate

생성물 1

HCID 178515486HCID 178515486, 화합물수율 15%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
120 °C

실험 절차

A mixture of 2H-1,2,4-triazol-3-amine (200 mg, 2.38 mmol, 1.00 equiv), acetic acid (3 mL), and ethyl 3-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-oxopropanoate (600 mg, 2.40 mmol, 1.01 equiv) was stirred for 24 hr at 120° C. and then concentrated to dryness. The resulting solid was washed with MeOH and collected by filtration. The solid was dissolved in 15 mL of NH4OH (aq.) and filtered. The filtrate was adjusted to pH 5 with HOAc. The resulting solid was collected by filtration and washed with water. The solid was dried to get 95 mg (15%) of 5-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-[1,2,4]triazolo[1,5-α]pyrimidin-7(4H)-one as a white solid.

후처리

  1. concentrationconcentrated to dryness
  2. washThe resulting solid was washed with MeOH
  3. filtrationcollected by filtration
  4. dissolutionThe solid was dissolved in 15 mL of NH4OH (aq.)
  5. filtrationfiltered
  6. filtrationThe resulting solid was collected by filtration
  7. washwashed with water
  8. customThe solid was dried

출처 및 근거

ORD 기록
ord-bde312b457114b68bc8a3ac5eae6bfc4
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09278973B2

연결된 노트

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