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Dimethylamine → Urea, N,N-dimethyl-N'-(4-(4-morpholinyl)-6-propyl-1,3,5-triazin-2-yl)-

HRID 1031870
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HRID 1031870 반응식
[CH3:1][NH:2][CH3:3].[O:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:15]=[C:14]([CH2:16][CH2:17][CH3:18])[N:13]=[C:12]([NH:19][C:20](=[O:28])OC3C=CC=CC=3)[N:11]=2)[CH2:6][CH2:5]1>ClCCl>[CH3:1][N:2]([CH3:3])[C:20]([NH:19][C:12]1[N:11]=[C:10]([N:7]2[CH2:6][CH2:5][O:4][CH2:9][CH2:8]2)[N:15]=[C:14]([CH2:16][CH2:17][CH3:18])[N:13]=1)=[O:28]
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참가 물질

4

반응물 2

HCID 674DimethylamineHCID 3080144Carbamic acid, (4-(4-morpholinyl)-6-propyl-1,3,5-triazin-2-yl)-, phenyl ester2회

생성물 1

HCID 3080162Urea, N,N-dimethyl-N'-(4-(4-morpholinyl)-6-propyl-1,3,5-triazin-2-yl)-수율 39.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A gaseous stream of dimethylamine is passed through a solution of 5 g (0.0145 mol) of phenyl (4-morpholino-6-propyl-1,3,5-triazin-2-yl)carbamate (compound 28) in 100 ml of anhydrous dichloromethane for three hours at a temperature of 20° C. The mixture is then allowed to stand for 12 hours. It is washed successively with a dilute sodium hydroxide solution and with water. The organic phase is dried over sodium sulfate and the solvent is evaporated under reduced pressure. The residue obtained crystallizes in a 50:50 mixture (v/v) of ethyl acetatehexane. 1.7 g of N,N-dimethyl-N'-(4-morpholino-6-propyl-1,3,5-triazin-2-yl)-urea is obtained.

후처리

  1. washIt is washed successively with a dilute sodium hydroxide solution and with water
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. customthe solvent is evaporated under reduced pressure
  4. customThe residue obtained
  5. customcrystallizes in a 50:50 mixture (v/v) of ethyl acetatehexane

출처 및 근거

ORD 기록
ord-f822b048092e43788f670238751587ca
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04956363

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