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Triethylamine → hexadecyl N-(4-methylpiperadinyl)carbamate

HRID 398744
ノート
印刷プレビュー

反応式

HRID 398744 の反応式
[NH2:1][N:2]1[CH2:7][CH2:6][CH:5]([CH3:8])[CH2:4][CH2:3]1.C(N(CC)CC)C.Cl[C:17]([O:19][CH2:20][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][CH3:35])=[O:18]>C(Cl)(Cl)Cl>[CH3:8][CH:5]1[CH2:6][CH2:7][N:2]([NH:1][C:17](=[O:18])[O:19][CH2:20][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][CH3:35])[CH2:3][CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 97633Cetyl chloroformateHCID 37335874-Methylpiperidin-1-amine

生成物 1

HCID 131720856hexadecyl N-(4-methylpiperadinyl)carbamate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

6.3 Grams of N-amino-4-methylpiperadine, 6.0 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 solution was slowly added dropwise 15.2 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 16.8 g of the desired product. m.p. 92° 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-b76e220b51e34a6095ee14f718de536d
出典データセット
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05817599

反応ノート

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