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

HRID 1380197노트

반응식

HRID 1380197 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 136067321-(3-Chloropropyl)-3-n-hexylurea수율 86.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2ddb5a103ba44923b1155c7c37ed4d7b
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04579947

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