Dodecylamine → 1-(3-Methoxybenzyl)-3-Dodecyl Thiourea

HRID 1356605

反応式

HRID 1356605 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].[CH3:14][O:15][C:16]1[CH:17]=[C:18]([CH:23]=[CH:24][CH:25]=1)[CH2:19][N:20]=[C:21]=[S:22]>C(O)C>[CH3:14][O:15][C:16]1[CH:17]=[C:18]([CH:23]=[CH:24][CH:25]=1)[CH2:19][NH:20][C: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])=[S:22]

参加物

4

反応物 2

HCID 13583DodecylamineHCID 1265123-Methoxybenzyl isothiocyanate

生成物 1

HCID 101334051-(3-Methoxybenzyl)-3-Dodecyl Thiourea

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
4 °C

実験手順

Dodecyl amine (4.89 g, 26.4 mmol) in 83 ml ethanol at 50° C. was reacted with 3-methoxybenzyl isothiocyanate (3.97 g, 22.1 mmol) for 6 h under N2 with stirring, and then poured into a 250 ml beaker. Performing this reaction at 40° C. led to a precipitate that was difficult to stir. Crystallization began as soon as the reaction started cooling below 50° C. The reaction mixture was cooled to 4° C. and the crystals were filtered off using Whatman 54 filter paper. The crystals were washed with 15 ml of ethanol. Combined filtrates were evaporated to dryness and taken up in 10 ml ethanol. Cooling the solution to −10° C. gave no crystals. The solution was evaporated to dryness and the solids were weighed. Material recovery was 98.7%, and yield of crystals was 7.62 g, or 94.4% of the theoretical yield. Calculated elemental analysis of 1-(3-methoxybenzyl)-3-dodecyl thiourea: C, 69.18; H, 9.95; N, 7.68; S, 8.79. Found: C, 69.65; H, 10.07; N, 7.67; S, 8.80.

後処理

  1. additionpoured into a 250 ml beaker
  2. customPerforming this reaction at 40° C.
  3. stirringto stir
  4. customCrystallization
  5. temperaturestarted cooling below 50° C
  6. filtrationthe crystals were filtered off
  7. filtrationfilter paper
  8. washThe crystals were washed with 15 ml of ethanol
  9. customCombined filtrates were evaporated to dryness
  10. temperatureCooling the solution to −10° C.
  11. customgave no crystals
  12. customThe solution was evaporated to dryness

出典と根拠

ORDレコード
ord-7b293dd9e1a64dd29a3f5bbf63221072
出典データセット
uspto-grants-2003_07
特許番号
US06586628B2

関連ノート

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