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Water → HCID 15524305, 화합물

HRID 324349
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HRID 324349 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:20]=[CH:21][C:22]=1[O:23][CH3:24])[CH2:5][NH:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:17]#[N:18])[CH:15]=2)[C:10](=[O:19])[NH:9][N:8]=1.[O:25]1[CH2:30][CH2:29][CH2:28][CH2:27][CH:26]1[O:31][CH2:32][CH2:33][CH2:34]Br.C(=O)([O-])[O-].[K+].[K+].O>CN1CCCC1=O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:20]=[CH:21][C:22]=1[O:23][CH3:24])[CH2:5][NH:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:17]#[N:18])[CH:15]=2)[C:10](=[O:19])[N:9]([CH2:34][CH2:33][CH2:32][O:31][CH:26]2[CH2:27][CH2:28][CH2:29][CH2:30][O:25]2)[N:8]=1
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6

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HCID 962WaterHCID 11430Potassium CarbonateHCID 27779882-(3-Bromopropoxy)tetrahydro-2H-pyranHCID 155243024-(3-Chloro-4-methoxybenzyl)amino-6-cyano-1(2H)-phthalazinone

생성물 1

HCID 15524305HCID 15524305, 화합물수율 70.6%

시약·촉매·용매 1

HCID 13387
N-methyl-2-pyrrolidone
용매

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온도
50 °C

실험 절차

4-(3-Chloro-4-methoxybenzyl)amino-6-cyano-1(2H)-phthalazinone (0.20 g) prepared in Example 21 was dissolved in 5 ml of N-methyl-2-pyrrolidinone, followed by the addition of 0.24 g of 3-bromopropyl 2-tetrahydropyranyl ether and 0.24 g of potassium carbonate. The obtained mixture was stirred at 50° C. for 4 hours and poured into water, followed by extraction with ethyl acetate. The organic phase was washed with water twice and with a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate and freed from the solvent by vacuum distillation. The residue was purified by silica gel column chromatography [solvent: n-hexane/ethyl acetate (1:1)] to give 0.20 g of the title compound as a yellow crystal.

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic phase was washed with water twice
  3. dry with materialwith a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate
  4. distillationfreed from the solvent by vacuum distillation
  5. customThe residue was purified by silica gel column chromatography [solvent: n-hexane/ethyl acetate (1:1)]

출처 및 근거

ORD 기록
ord-9d4e55a3a57c448cabd895fb9c940f58
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06218392B1

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