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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 54562765, 화합물

HRID 362920
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인쇄 미리보기

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HRID 362920 반응식
[CH3:1][N:2]([CH3:15])[C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=O)=[C:5]([N+:12]([O-:14])=[O:13])[CH:4]=1.[NH2:16][CH:17]1[CH2:22][CH2:21][N:20]([CH:23]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH2:19][CH2:18]1.CCN=C=NCCCN(C)C.Cl>CN(C1C=CN=CC=1)C.C(Cl)Cl>[CH3:15][N:2]([CH3:1])[C:3]1[CH:11]=[CH:10][C:6]([C:7]([NH:16][CH:17]2[CH2:22][CH2:21][N:20]([CH:23]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[CH2:19][CH2:18]2)=[O:9])=[C:5]([N+:12]([O-:14])=[O:13])[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 128755351-(Diphenylmethyl)-4-piperidinamineHCID 54252267HCID 54252267, 화합물

생성물 1

HCID 54562765HCID 54562765, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 6344
Dichloromethane
용매
2회

실험 절차

Step 3): The mixture of 4-dimethylamino-2-nitrobenzoic acid (4.20 g, 20 mmol), 4-amino-1-diphenylmethylpiperidine (5.33 g, 20 mmol). EDCl (4.00 g, 21 mmol) and DMAP (2.45 g, 20 mmol) in CH2Cl2 (60 ml) was stirred at room temperature for 17.5 hours. The reaction mixture was diluted with CH2Cl2, washed with H2O and brine. The organic layer was dried over MgSO4 and concentrated under vacuum. The residue was purified with chromatography on SiO2 (50% AcOEt in hexane) and recrystallized from AcOEt to obtain 4-dimethylamino-2-nitro-N-(1-diphenylmethylpiperidin-4-yl)benzamide. 5.44 g (59%): mp 183° C.

후처리

  1. washwashed with H2O and brine
  2. dry with materialThe organic layer was dried over MgSO4
  3. concentrationconcentrated under vacuum
  4. customThe residue was purified with chromatography on SiO2 (50% AcOEt in hexane)
  5. customrecrystallized from AcOEt

출처 및 근거

ORD 기록
ord-2ca58f434a1548cb83a3e37fce4768f0
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05872115

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