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Potassium Carbonate → HCID 9950805, 화합물

HRID 496554
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HRID 496554 반응식
[CH3:1][C:2]1[O:6][N:5]=[C:4]([C:7]2[N:11]3[NH:12][C:13](=[O:20])[C:14]4[C:19]([C:10]3=[N:9][CH:8]=2)=[CH:18][CH:17]=[CH:16][CH:15]=4)[CH:3]=1.[H-].[Na+].C(=O)([O-])[O-].[K+].[K+].Cl.Cl[CH2:31][C:32]1[N:33]=[N:34][N:35]([CH3:37])[CH:36]=1>CN(C=O)C.O>[CH3:1][C:2]1[O:6][N:5]=[C:4]([C:7]2[N:11]3[N:12]=[C:13]([O:20][CH2:31][C:32]4[N:33]=[N:34][N:35]([CH3:37])[CH:36]=4)[C:14]4[C:19]([C:10]3=[N:9][CH:8]=2)=[CH:18][CH:17]=[CH:16][CH:15]=4)[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 24758Sodium hydrideHCID 223215554-(chloromethyl)-1-methyl-1H-1,2,3-triazole hydrochlorideHCID 22321557HCID 22321557, 화합물

생성물 1

HCID 9950805HCID 9950805, 화합물수율 62%

시약·촉매·용매 2

HCID 962Water
용매
HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

3-(5-Methylisoxazol-3-yl)imidazo[2,1-a]phthalazin-6-one (100 mg, 0.375 mmol) was suspended in DMF (5 ml) and sodium hydride (60% dispersion in oil, 33 mg, 0.83 mmol) was added. After stirring at room temperature for 10 minutes potassium carbonate (50 mg, 0.36 mmol) was added, followed by 4-chloromethyl-1-methyl triazole hydrochloride (69 mg, 0.41 mmol). The solution was heated at 80° C. for 4 hours, then cooled and poured into water. The solid product was filtered off and washed with water and hexane. The solid was recrystallised from ethyl acetate/hexane to yield the title compound (83 mg, 62%), 1H NMR (360 MHz, CDCl3) 2.55 (3H, s), 4.11 (3H, s), 5.75 (2H, s), 6.72 (1H, s), 7.67 (1H, t), 7.86 (1H, t), 7.99 (1H, s), 8.17 (2H, d), 8.51 (1H, d); MS+362 [MH]+.

후처리

  1. additionwas added
  2. temperaturecooled
  3. filtrationThe solid product was filtered off
  4. washwashed with water and hexane
  5. customThe solid was recrystallised from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-75a227f680694b44988544ec3f1fe68a
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06946461B2

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