Enantholactam → HCID 178443232、化合物

HRID 461020

反応式

HRID 461020 の反応式
[C:1]1(=O)[NH:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.P(Cl)(Cl)(Cl)=O.[CH2:15]([NH2:27])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]>C1C=CC=CC=1>[CH2:15]([N:27]=[C:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][NH:8]1)[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]

参加物

5

反応物 3

HCID 12657EnantholactamHCID 13583DodecylamineHCID 24813Phosphorus oxychloride

生成物 1

HCID 178443232HCID 178443232、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To 28.3 g (0.223 mole) of an enantholactam in 250 ml of benzene is added 34.1 g (0.223 mole) of phosphorous oxychloride over 30 minutes. The mixture is stirred at room temperature for 4 hours after which 41.2 g (0.223 mole) of dodecylamine is added. The reaction mixture is stirred at room temperature for 1 hour and refluxed for 4 hours then allowed to stand overnight. The resulting precipitate is washed with benzene, and the benzene wash is extracted with aqueous 2 N hydrochloric acid and combined with the precipitate. The combined fractions are made alkaline with 2N sodium hydroxide, extracted into ether-methylene chloride, dried and recrystallized from isopropyl alcohol to give 2-dodecyliminooctahydroazocine.

後処理

  1. additionis added
  2. temperaturerefluxed for 4 hours
  3. waitto stand overnight
  4. washThe resulting precipitate is washed with benzene
  5. washthe benzene wash
  6. extractionis extracted with aqueous 2 N hydrochloric acid
  7. extractionextracted into ether-methylene chloride
  8. customdried
  9. customrecrystallized from isopropyl alcohol

出典と根拠

ORDレコード
ord-2b6fff81fdb74047b512baa955c5d4e9
出典データセット
uspto-grants-1977_12
特許番号
US04061746

関連ノート

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