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Methanol → HCID 59355185, 화합물

HRID 1023494
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HRID 1023494 반응식
[CH3:1][N:2]([CH3:11])[CH2:3][CH2:4][NH:5][CH2:6][C:7]([CH3:10])([NH2:9])[CH3:8].C1N=CN([C:17](N2C=NC=C2)=[O:18])C=1.CO>C(Cl)Cl>[CH3:11][N:2]([CH3:1])[CH2:3][CH2:4][N:5]1[CH2:6][C:7]([CH3:8])([CH3:10])[NH:9][C:17]1=[O:18]
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참가 물질

5

반응물 3

HCID 887MethanolHCID 682631,1'-CarbonyldiimidazoleHCID 59355176HCID 59355176, 화합물

생성물 1

HCID 59355185HCID 59355185, 화합물수율 2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of N1-(2-(dimethylamino)ethyl)-2-methylpropane-1,2-diamine (23.2 mmol) in CH2Cl2 (50 ml) was added CDI (4.51 g, 27.8 mmol). The solution was stirred for 20 h, concentrated in vacuo, the resulting residue suspended in 800 ml diethyl ether, washed with 3× 200 ml 1M Na2CO3, 200 ml sat. NaCl, dried on MgSO4, and concentrated in vacuo. Flash chromatography (2.5%→20% MeOH:CH2Cl2) afforded the title compound as a clear oil (79.3 mg, 0.428 mmol, 2%) as well as additional material heavily contaminated with imidazole g). 1H NMR (CDCl3, 400 MHz) δ 1.24 (s, 6H), 2.23 (s, 6H), 2.41 (m, 2H), 3.24 (s, 2H), 3.34 (m, 2H), 4.96 (s, 1H). ESI/APCI (pos) expected for C9H19N3O: 185.15. Found: 186 (MH+).

후처리

  1. concentrationconcentrated in vacuo
  2. washwashed with 3× 200 ml 1M Na2CO3, 200 ml sat. NaCl
  3. customdried on MgSO4
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ad9a73bc5f214367965ceee3a50ae5c8
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722715B2

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