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Ammonium Acetate → HCID 59699556, 화합물

HRID 901242
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HRID 901242 반응식
C([O-])(=[O:3])C.[NH4+].Cl[C:7]1[C:16]([C:17]#[N:18])=[C:15]([Cl:19])[C:14]2[C:9](=[N:10][CH:11]=[CH:12][CH:13]=2)[N:8]=1>C(O)(=O)C>[Cl:19][C:15]1[C:14]2[C:9](=[N:10][CH:11]=[CH:12][CH:13]=2)[NH:8][C:7](=[O:3])[C:16]=1[C:17]#[N:18]
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참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 59699635HCID 59699635, 화합물

생성물 1

HCID 59699556HCID 59699556, 화합물수율 48%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
140 °C

실험 절차

Ammonium acetate (6.81 g, 88.37 mmol) was added to a suspension of 2,4-Dichloro-[1,8]-naphthyridine-3-carbonitrile (30) in acetic acid at room temperature and heated at 140° C. for 45 min. The solution was cooled and poured into ice water. The solids formed were filtered, washed with cold water and suspended in saturated sodium bicarbonate solution. After stirring overnight at room temperature, the solids were filtered, washed by cold water, and dried at room temperature under vacuum to yield 8.0 g (48%) of 4-chloro-2-oxo-1,2-dihydro-[1,8]-naphthyridine-3-carbonitrile (31) as white solids. MP: 310° C.; 1H-NMR (DMSO-d6): δ 7.58 (dd, J=4.4, 8.0 Hz, 1H), 8.50 (d, J=2.0, 8.0 Hz, 1H), 8.83 (dd, J=4.4, 1.6 Hz, 1H), 13.03 (S, 1H); EIMS: 206 (M+1).

후처리

  1. temperatureThe solution was cooled
  2. customThe solids formed
  3. filtrationwere filtered
  4. washwashed with cold water
  5. filtrationthe solids were filtered
  6. washwashed by cold water
  7. customdried at room temperature under vacuum

출처 및 근거

ORD 기록
ord-d8bd9ea4e24b41c69a08579367244d5c
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07361760B2

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