Dodecylamine → HCID 18980712、化合物

HRID 2392916ノート

反応式

HRID 2392916 の反応式
[CH2:1]([NH2:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].Cl[CH2:15][CH:16]([OH:36])[CH2:17][N:18]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])[CH2:19][CH:20]([OH:23])[CH2:21]Cl>C1(C)C(C)=CC=CC=1>[OH:36][CH:16]([CH2:17][N:18]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])[CH2:19][CH:20]([OH:23])[CH2:21][NH:13][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH2:15][NH:13][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

参加物

4

反応物 2

HCID 13583DodecylamineHCID 189807231,1'-(Dodecylazanediyl)bis(3-chloropropan-2-ol)

生成物 1

HCID 18980712HCID 18980712、化合物収率 49.4%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒2 回

反応条件

温度
80 °C

実験手順

A reactor was charged with 286.3 g (1.54 moles) of dodecylamine and 90 g of xylene, and the contents were heated to 80° C. To the contents, a solution with 57 g (0.15 mole) of N,N-bis(3-chloro-2-hydroxypropyl)dodecylamine dissolved in 50 g of xylene was added dropwise over 1.5 hours. The resultant mixture was aged further for 4 hours. Thereafter, xylene was distilled off under reduced pressure, and unreacted dodecylamine was then distilled off at 100° C. and 0.5 mmHg. The residue was added with 500 ml of hexane and 2000 ml of acetone to be dissolved therein. The solution was then subjected to extraction and washing with a mixture of 500 ml of xylene and 500 ml of 5% aqueous sodium hydroxide. Thereafter, a xylene layer was taken out and concentrated, thereby obtaining 49.5 g (yield: 48%) of 15,19-dihydroxy-17-dodecyl-13,17,21-triazatritriacontane represented by the following formula. ##STR10##

後処理

  1. additionwas added dropwise over 1.5 hours
  2. distillationThereafter, xylene was distilled off under reduced pressure, and unreacted dodecylamine
  3. distillationwas then distilled off at 100° C.
  4. additionThe residue was added with 500 ml of hexane and 2000 ml of acetone
  5. dissolutionto be dissolved
  6. extractionThe solution was then subjected to extraction
  7. washwashing with a mixture of 500 ml of xylene and 500 ml of 5% aqueous sodium hydroxide
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-b928c7e3fe0243fa921325ee854becf2
出典データセット
uspto-grants-1998_09
特許番号
US05801270

反応ノート

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