Triethylamine → 2-[3-(4-Methylpiperazino)-3-oxopropyl]phenyl N-octadecylcarbamate

HRID 1250764노트

반응식

HRID 1250764 반응식
C(N(CC)CC)C.[CH2:8]([N:26]=[C:27]=[O:28])[CH2:9][CH2:10][CH2:11][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][CH3:25].[OH:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[CH2:36][CH2:37][C:38]([N:40]1[CH2:45][CH2:44][N:43]([CH3:46])[CH2:42][CH2:41]1)=[O:39]>C(Cl)Cl>[CH2:8]([NH:26][C:27](=[O:28])[O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[CH2:36][CH2:37][C:38]([N:40]1[CH2:45][CH2:44][N:43]([CH3:46])[CH2:42][CH2:41]1)=[O:39])[CH2:9][CH2:10][CH2:11][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][CH3:25]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 66988Octadecyl isocyanateHCID 185202573-(2-Hydroxyphenyl)-1-(4-methylpiperazino)-1-propanone

생성물 1

HCID 98074162-[3-(4-Methylpiperazino)-3-oxopropyl]phenyl N-octadecylcarbamate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triethylamine (0.62 mld) and octadecyl isocyanate (1.40 ml) were added to a solution containing 3-(2-hydroxyphenyl)-1-(4-methylpiperazino)-1-propanone (1.00 g) in methylene chloride (10 ml) and stirred for 4 hours at room temperature. The insoluble matters were filtrated out and washed with chloroform. The filtrate and washings were combined and the i mixture was washed with saturated sodium hydrogencarbonate aqueous solution and brine successively, dried over sodium sulfate anhydride, and concentrated. The residue was purified by silica gel column chromatography (silica gel 50 g, chloroform:methanol=50:1), thereby yielding the entitled compound (2.05 g) as white solid.

후처리

  1. filtrationThe insoluble matters were filtrated out
  2. washwashed with chloroform
  3. washthe i mixture was washed with saturated sodium hydrogencarbonate aqueous solution and brine successively
  4. dry with materialdried over sodium sulfate anhydride
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (silica gel 50 g, chloroform:methanol=50:1)

출처 및 근거

ORD 기록
ord-b25c683f6b8e426891fd568f90df0835
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06339154B1

반응 노트

불러오는 중…