Potassium Carbonate → 3-[4-(3-chloro-4-methoxyanilino)-6-cycloheptylamino-1,3,5-triazin-2-yloxy]-2-ethyl-4H-4-pyranone

HRID 719429

반응식

HRID 719429 반응식
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[C:11]([Cl:17])[CH:10]=2)[N:5]=[C:4]([NH:18][CH:19]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]2)[N:3]=1.[CH2:26]([C:28]1[O:29][CH:30]=[CH:31][C:32](=[O:35])[C:33]=1[OH:34])[CH3:27].C([O-])([O-])=O.[K+].[K+]>CN(C)C=O.O>[Cl:17][C:11]1[CH:10]=[C:9]([CH:14]=[CH:13][C:12]=1[O:15][CH3:16])[NH:8][C:6]1[N:5]=[C:4]([NH:18][CH:19]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]2)[N:3]=[C:2]([O:34][C:33]2[C:32](=[O:35])[CH:31]=[CH:30][O:29][C:28]=2[CH2:26][CH3:27])[N:7]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 21059Ethyl MaltolHCID 218970216-chloro-N-(3-chloro-4-methoxyphenyl)-N'-cycloheptyl-[1,3,5]triazine-2,4-diamine

생성물 1

HCID 115403443-[4-(3-chloro-4-methoxyanilino)-6-cycloheptylamino-1,3,5-triazin-2-yloxy]-2-ethyl-4H-4-pyranone

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A mixture of 133 (0.3 g, 0.78 mmol), 2-ethyl-3-hydroxy-4H-pyran-4-one (0.11 g, 0.78 mmol) and K2CO3 (0.54 g, 3.91 mmol) in dimethylformamide (15 mL) was stirred at 80° C. for 6 hours under nitrogen atmosphere. After completion of the reaction the mixture was cooled to 25° C. and diluted with water (50 mL). The precipitated solid was filtered off and dried under vacuum to afford the title compound E19 as an off-white solid (0.2 g, 52%). mp 124–126° C.; HPLC: Inertsil ODS 3V (250×4.6 mm) 5 microns 50:50 [0.01 M KH2PO4 (0.1% TFA):CH3CN], 223 nm, Rt 18.47 min, 98.18% purity); MS (CI): m/z 486 (M+, 100), 382 (90).

후처리

  1. customAfter completion of the reaction the mixture
  2. temperaturewas cooled to 25° C.
  3. filtrationThe precipitated solid was filtered off
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-93c39c07efde46d7bf1bcbc537206d8d
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07132423B2

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