Triethylamine → HCID 13534703, 화합물

HRID 4361

반응식

HRID 4361 반응식
Cl.[NH2:2][N:3]1[CH2:8][CH:7]=[CH:6][CH2:5][CH2:4]1.C(N(CC)CC)C.[F:16][C:17]1[CH:18]=[C:19]([N:23]=[C:24]=[O:25])[CH:20]=[CH:21][CH:22]=1>C(Cl)Cl>[F:16][C:17]1[CH:18]=[C:19]([NH:23][C:24]([NH:2][N:3]2[CH2:4][CH:5]=[CH:6][CH2:7][CH2:8]2)=[O:25])[CH:20]=[CH:21][CH:22]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 1230643-Fluorophenyl isocyanateHCID 193760471,2,3,6-Tetrahydropyridin-1-amine hydrochloride

생성물 1

HCID 13534703HCID 13534703, 화합물수율 60.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of N-amino-1,2,3,6-tetrahydropyridine hydrochloride (1.346 g) and triethylamine (1.012 g) in dry methylene chloride (40 ml) was added a solution of 3-fluorophenyl isocyanate (1.37 g) in dry methylene chloride under ice-bath cooling. After stirring for one hour, the reaction mixture was evaporated to dryness. The residue was extracted with ethyl acetate (100 ml). The extract was washed with water, evaporated to dryness and recystallized from ethyl acetate to give N-[[(3-fluorophenyl)carbamoyl]amino]-1,2,3,6-tetrahydropyridine (1.43 g). mp: 136.5°-138.5° C.

후처리

  1. temperaturecooling
  2. customthe reaction mixture was evaporated to dryness
  3. extractionThe residue was extracted with ethyl acetate (100 ml)
  4. washThe extract was washed with water
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-15946ac52f84452daf9d7ce6d8f8fe10
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725608

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