Hydrochloric Acid → Urea, N'-(2,4-difluorophenyl)-N-heptyl-N-(5-hydroxypentyl)-

HRID 486083노트

반응식

HRID 486083 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[F:15][C:16]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:17]=1[N:23]=[C:24]=[O:25].Cl>C(Cl)Cl>[F:15][C:16]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:17]=1[NH:23][C:24](=[O:25])[N:7]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][OH:1]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 5932582,4-Difluorophenyl isocyanateHCID 10352800N-(5-hydroxypentyl) heptylamine

생성물 1

HCID 11725825Urea, N'-(2,4-difluorophenyl)-N-heptyl-N-(5-hydroxypentyl)-수율 96.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Part C. To a solution of N-(5-hydroxypentyl)-N-heptylamine (11.65 g, 0.0578 mol) in methylene chloride (75 mL) under a nitrogen atmosphere cooled to 0°, 2,4-difluorophenylisocyanate (8.97 g, 0.0578 mol) was added slowly. The reaction mixture was stirred for 1 hour, poured into 1 N aqueous HCl (200 mL) and was extracted with ethyl acetate (300 mL). The combined organic extracts were washed with water and brine, then dried over magnesium sulfate and concentrated to give N'-(2,4-difluorophenyl)-N-heptyl-N-5-hydroxypentylurea as a pale yellow oil (20.0 g, 0.056 mol). 1H NMR (CDCl3) δ8.03 (m,1H), 6.88-6.59 (m,2H), 6.45 (bs,1H), 3.68 (t,2H,J=6.7 Hz).

후처리

  1. extractionwas extracted with ethyl acetate (300 mL)
  2. washThe combined organic extracts were washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-98994deae8464be090787872c4e331c1
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05290801

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