Triethylamine → hexadecyl N-(2-piperidinoethyl)carbamate

HRID 398742

反応式

HRID 398742 の反応式
[NH2:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][CH2:7][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>[N:4]1([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])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 33944N-(2-Aminoethyl)piperidineHCID 97633Cetyl chloroformate

生成物 1

HCID 18968674hexadecyl N-(2-piperidinoethyl)carbamate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

7.3 Grams of N-(2-aminoethyl)piperidine, 5.2 g of triethylamine and 100 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 15.8 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 methanol to obtain 16.3 g of the desired product. m.p. 48° 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 methanol

出典と根拠

ORDレコード
ord-07dc6c34c40d477094e8aae9a9913e20
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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