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3-Isocyanatopyridine → US9296747, Example 3

HRID 930502
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HRID 930502 반응식
[C:1]1([NH:7][C:8]2[N:9]=[CH:10][C:11]3[CH2:17][NH:16][CH2:15][CH2:14][C:12]=3[N:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N:18]([C:21]1[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=1)=[C:19]=[O:20]>C(Cl)Cl>[NH:7]([C:8]1[N:9]=[CH:10][C:11]2[CH2:17][N:16]([C:19]([NH:18][C:21]3[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=3)=[O:20])[CH2:15][CH2:14][C:12]=2[N:13]=1)[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
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참가 물질

4

반응물 2

HCID 27604933-IsocyanatopyridineHCID 104609480N-phenyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-2-amine

생성물 1

HCID 118970906US9296747, Example 3

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of N-phenyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-2-amine, Intermediate 6 (75 mg, 0.33 mmol), 3-isocyanatopyridine (41.8 mg, 0.35 mmol) in CH2Cl2 (1.5 mL) was stirred at room temperature for 1 hour. After 1 hour the reaction mixture was diluted with CH2Cl2 and washed with sat. aqueous NaHCO3(aq). The organic phase was collected, dried and concentrated. The residue was dissolved in CH2Cl2 and washed with 3% aqueous LiCl solution and water. The organic phase was collected, dried and concentrated to give the title compound (45.9 mg).

후처리

  1. washwashed with sat. aqueous NaHCO3(aq)
  2. customThe organic phase was collected
  3. customdried
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in CH2Cl2
  6. washwashed with 3% aqueous LiCl solution and water
  7. customThe organic phase was collected
  8. customdried
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8fb5bbed33ea4f298a56f5d494fdd45f
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296747B1

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