Sodium Hydroxide → N2-(3-chloro-4-methoxyphenyl)-N4-cycloheptyl-6-(4-methylpiperzino)-1,3,5-triazine-4,2-diamine

HRID 719428

반응식

HRID 719428 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.[CH3:26][N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1.[OH-].[Na+]>O1CCOCC1.O>[Cl:17][C:11]1[CH:10]=[C:9]([NH:8][C:6]2[N:5]=[C:4]([NH:18][CH:19]3[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)[N:3]=[C:2]([N:30]3[CH2:31][CH2:32][N:27]([CH3:26])[CH2:28][CH2:29]3)[N:7]=2)[CH:14]=[CH:13][C:12]=1[O:15][CH3:16]

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 531671-MethylpiperazineHCID 218970216-chloro-N-(3-chloro-4-methoxyphenyl)-N'-cycloheptyl-[1,3,5]triazine-2,4-diamine

생성물 1

HCID 21057791N2-(3-chloro-4-methoxyphenyl)-N4-cycloheptyl-6-(4-methylpiperzino)-1,3,5-triazine-4,2-diamine

시약·촉매·용매 2

HCID 962Water용매2회HCID 312751,4-Dioxane용매2회

반응 조건

온도
25 °C

실험 절차

To a solution of 133 (0.5 g, 1.31 mmol) in 1,4-dioxane (5 mL) was added slowly a solution of 1-methylpiperizine (0.13 g, 1.31 mmol) in 1,4-dioxane (5 mL) followed by 2.5 N sodium hydroxide solution (0.5 mL, 1.31 mmol) and water (1.2 mL). The mixture was heated to reflux for 2.5–3 hours with stirring under nitrogen atmosphere and then cooled to 25° C. and diluted with water (10 mL). The mixture was then stirred for 10–15 min., the precipitated solid was filtered off and dried under vacuum to afford the title compound E18 as an off-white solid (0.5 g, 86%). mp 120–122° C.; HPLC: Inertsil ODS 3V (250×4.6 mm) 5 microns 65: 35 [0.01 M KH2PO4 (0.1% TFA):CH3CN], 223 nm, Rt 10.23 min, 98.50% purity); MS (CI): m/z 446 (M+H, 100), 375 (25).

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 2.5–3 hours
  3. stirringThe mixture was then stirred for 10–15 min.
  4. filtrationthe precipitated solid was filtered off
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-c0b2880d939346209c1fd1b4296e210c
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07132423B2

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