Triethylamine → hexadecyl N-(2-morpholinoethyl)carbamate

HRID 398743

反応式

HRID 398743 の反応式
[NH2:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][O:7][CH2:6][CH2:5]1.C(N(CC)CC)C.Cl[C:18]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])=[O:19]>C(Cl)(Cl)Cl>[O:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH2:2][NH:1][C:18](=[O:19])[O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])[CH2:5][CH2:6]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 97633Cetyl chloroformateHCID 4082852-Morpholinoethylamine

生成物 1

HCID 18968659hexadecyl N-(2-morpholinoethyl)carbamate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

8.6 Grams of N-(2-aminoethyl)morpholine, 7.2 g of triethylamine and 120 ml of chloroform were charged in a flask equipped with a stirrer, a condenser and a calcium chloride drying tube and stirred with ice cooling. To the resulting solution was slowly added dropwise 18.2 g of hexadecyl chloroformate. After completion of the addition, the temperature of the solution was returned to room temperature, followed by refluxing with heating for 0.5 hour. The reaction mixture was cooled to room temperature, washed with water, dried over anhydrous magnesium sulfate and, then, concentrated under reduced pressure. The residue was recrystallized from acetonitrile to obtain 21.1 g of the desired product. m.p. 65° C.

後処理

  1. customequipped with a stirrer, a condenser and a calcium chloride drying tube
  2. additionAfter completion of the addition
  3. customwas returned to room temperature
  4. temperatureby refluxing
  5. temperaturewith heating for 0.5 hour
  6. washwashed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-8468dbbf0db54cf2839884f6fb65888e
出典データセット
uspto-grants-1998_10
特許番号
US05817599

関連ノート

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