Triethylamine → 1-(3-Chloropropyl)-3-n-hexylurea

HRID 543184ノート

反応式

HRID 543184 の反応式
C(N(CC)CC)C.Cl.[Cl:9][CH2:10][CH2:11][CH2:12][NH2:13].[CH2:14]([N:20]=[C:21]=[O:22])[CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]>C(Cl)Cl>[Cl:9][CH2:10][CH2:11][CH2:12][NH:13][C:21]([NH:20][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:22]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 75659Hexyl isocyanateHCID 114690951-Propanamine, 3-chloro-, hydrochloride

生成物 1

HCID 136067321-(3-Chloropropyl)-3-n-hexylurea収率 86.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Triethylamine (35 g; 35 mmole) was slowly added to a mixture of chloropropylamine hydrochloride (39 g; 0.3 mol), n-hexyl isocyanate (38.2 g; 0.3 mole) and methylene chloride (500 ml). The resulting solution was stirred for one hour, and then the solvent was removed in vacuo. The residue was treated with ether, and the colorless solid was filtered off. The ether solution was then washed with water, dried (magnesium sulfate) and concentrated to give pure 1-(3-chloropropyl)-3-n-hexylurea (57.0 g; 86% yield) as colorless crystals, m.p. 48°-50° C.

後処理

  1. customthe solvent was removed in vacuo
  2. additionThe residue was treated with ether
  3. filtrationthe colorless solid was filtered off
  4. washThe ether solution was then washed with water
  5. dry with materialdried (magnesium sulfate)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-2e627a3b779940e7a096bbba2d2c5c27
出典データセット
uspto-grants-1987_04
特許番号
US04661481

反応ノート

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