Triethylamine → HCID 13534703、化合物

HRID 4361

反応式

HRID 4361 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 13534703HCID 13534703、化合物収率 60.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-15946ac52f84452daf9d7ce6d8f8fe10
出典データセット
uspto-grants-1988_02
特許番号
US04725608

関連ノート

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