Dimethyloctadecylamine → HCID 178419186、化合物

HRID 649501

反応式

HRID 649501 の反応式
[BH3:1].C(N(CC)CC)C.[CH3:9][N:10]([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])[CH3:11]>>[BH3:1].[CH2:12]([N:10]([CH3:11])[CH3:9])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29]

参加物

3

反応物 2

HCID 15365DimethyloctadecylamineHCID 264094borane;N,N-diethylethanamine

生成物 1

HCID 178419186HCID 178419186、化合物

実験手順

To a one-neck round-bottom flask (with thermometer well), equipped with magnetic stirrer, distillation head and condenser, were added 3.87 g. (0.0336 mol) triethylamine borane and 10.0 g. (0.0336 mol) N,N-dimethyloctadecylamine. With stirring, the flask was heated to slowly distill off triethylamine (max. reaction temp. 240° C). After removing 3.2 ml. of triethylamine, heating was interrupted and 10 ml. toluene added to the cooled reaction flask. Distillation was continued until 9.0 ml. were removed (last few drops removed under 15-20 mm. vacuum). The solid in the reaction flask was recrystallized from 30°-60° petroleum ether yielding 7.58 g. (72%) of white crystals, mp 56°-57.5° C. IR (Nujol) 2300 cm-1 (B-H). Anal. Calcd for C20H46BN: C, 77.14; H, 14.89; B, 3.47; N, 4.50. Found C, 77.21; H, 14.90; B, 3.36; N, 4.50.

後処理

  1. customTo a one-neck round-bottom flask (with thermometer well), equipped with magnetic stirrer
  2. distillationdistillation head and condenser
  3. additionwere added 3.87 g
  4. temperaturethe flask was heated
  5. distillationto slowly distill off triethylamine (max. reaction temp. 240° C)
  6. customAfter removing 3.2 ml
  7. temperatureof triethylamine, heating
  8. additiontoluene added to the cooled reaction flask
  9. distillationDistillation
  10. customwere removed
  11. custom(last few drops removed under 15-20 mm. vacuum)
  12. customThe solid in the reaction flask was recrystallized from 30°-60° petroleum ether yielding 7.58 g

出典と根拠

ORDレコード
ord-8dd602ee0f1a42b3b511d313ef80c80b
出典データセット
uspto-grants-1988_04
特許番号
US04740504

関連ノート

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