Aminoethylpiperazine → 2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy-N-[2-(1-piperazinyl)ethyl]acetamide

HRID 1198908노트

반응식

HRID 1198908 반응식
[Cl:1][C:2]1[CH:14]=[C:13]([C:15]2[CH:16]([CH3:22])[NH:17][C:18](=[O:21])[NH:19][N:20]=2)[CH:12]=[CH:11][C:3]=1[O:4][CH2:5][C:6]([O:8]CC)=O.[NH2:23][CH2:24][CH2:25][N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1>C(O)C>[Cl:1][C:2]1[CH:14]=[C:13]([C:15]2[CH:16]([CH3:22])[NH:17][C:18](=[O:21])[NH:19][N:20]=2)[CH:12]=[CH:11][C:3]=1[O:4][CH2:5][C:6]([NH:23][CH2:24][CH2:25][N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)=[O:8]

참가 물질

4

반응물 2

HCID 8795AminoethylpiperazineHCID 14370696Ethyl alpha-[2-chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetate

생성물 1

HCID 143707002-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy-N-[2-(1-piperazinyl)ethyl]acetamide수율 68.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4.0 g of ethyl α-[2-chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetate (prepared as described in Example 5) and 1.59 g of N-(2-aminoethyl)piperazine were added to 50 ml of ethanol, and the mixture was heated under reflux for 60 hours. The mixture was then cooled, after which the crystals which precipitated were collected by filtration and then recrystallized from ethanol to give 3.44 g of the title compound as pale yellow prisms melting at 208°-210° C.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 60 hours
  3. temperatureThe mixture was then cooled
  4. customafter which the crystals which precipitated
  5. filtrationwere collected by filtration
  6. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-5605edfe49b14265bdec99415c7d4293
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04898862

반응 노트

불러오는 중…