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Ammonia → HCID 178517686, 화합물

HRID 1480832
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HRID 1480832 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([C:16](/[CH:19]=[CH:20]/OCC)=[CH:17][N:18]=1)[C:12](OC)=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC1C=CC(S(O)(=O)=O)=CC=1.O.[NH3:36]>>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16]([CH:19]=[CH:20][N:36]=[C:12]2[OH:13])=[CH:17][N:18]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 222AmmoniaHCID 521998p-Toluenesulfonic acid monohydrateHCID 89996003HCID 89996003, 화합물

생성물 1

HCID 178517686HCID 178517686, 화합물수율 97%

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온도
80 °C

실험 절차

(E)-methyl 2-(benzyloxy)-5-(2-ethoxyvinyl)isonicotinate (Preparation 85, 1.2 g, 3.83 mmol) was dissolved in methanolic ammonia (7M, 28 mL) in 3 microwave tubes. The reaction mixture was sealed and heated to 80° C. for 3 days. The reaction mixture was concentrated in vacuo. The residue was dissolved in toluene (30 mL) and pTsOH.H2O (150 mg, 0.789 mmol) was added. The reaction mixture was heated at 90° C. for 2 hours. The reaction mixture was filtered and dried under vacuum, to give the title compound (937 mg, 97%).

후처리

  1. customThe reaction mixture was sealed
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionThe residue was dissolved in toluene (30 mL)
  4. temperatureThe reaction mixture was heated at 90° C. for 2 hours
  5. filtrationThe reaction mixture was filtered
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-6bd9ddb382634eafa61904013899a8ec
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409907B2

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