2-Morpholinoethylamine → 6-[3-Chloro-4-(2-morpholinoethyl)carbamoylmethoxyphenyl]-5-methyl-4,5-dihydro-1,2,4-triazin-3(2H)-one

HRID 1198906노트

반응식

HRID 1198906 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][O:29][CH2:28][CH2:27]1>O>[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])[NH:23][CH2:24][CH2:25][N:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1

참가 물질

4

반응물 2

HCID 4082852-MorpholinoethylamineHCID 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 147267386-[3-Chloro-4-(2-morpholinoethyl)carbamoylmethoxyphenyl]-5-methyl-4,5-dihydro-1,2,4-triazin-3(2H)-one수율 40%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixure of 507 mg 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 407 mg of N-(2-aminoethyl)morpholine was stirred at 110°-115° C. (bath temperature) for 1 hour. The mixture was cooled and poured into water. The crystals which precipitated were collected by filtration. These crude crystals were recrystallized from a mixture of methanol and ethyl acetate to give 255 mg of the title compound as a white powder melting at 179°-181° C. (with decomposition). The filtrate was extracted with ethyl acetate, dried and concentrated by evaporation under reduced pressure, followed by trituration of the residue with ethyl acetate to give a further 91 mg of the title compound as crystals.

후처리

  1. temperatureThe mixture was cooled
  2. customThe crystals which precipitated
  3. filtrationwere collected by filtration
  4. customThese crude crystals were recrystallized from a mixture of methanol and ethyl acetate

출처 및 근거

ORD 기록
ord-9310b00234fe4e2a9323bb45b2d9d691
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04898862

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