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Pyridine → HCID 70055165, 화합물

HRID 583374
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HRID 583374 반응식
[CH3:1][O:2][C:3](=[O:32])[C:4]1[CH:9]=[C:8]([CH2:10]Br)[CH:7]=[C:6]([CH3:12])[C:5]=1[N:13]([CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[S:14]([C:17]1[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=1)(=[O:16])=[O:15].[CH2:33]([NH:35][CH2:36][CH3:37])[CH3:34].N1C=CC=CC=1>ClCCl>[CH3:1][O:2][C:3](=[O:32])[C:4]1[CH:9]=[C:8]([CH2:10][N:35]([CH2:36][CH3:37])[CH2:33][CH3:34])[CH:7]=[C:6]([CH3:12])[C:5]=1[N:13]([CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[S:14]([C:17]1[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=1)(=[O:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 8021DiethylamineHCID 70053591HCID 70053591, 화합물

생성물 1

HCID 70055165HCID 70055165, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 518.4 mg (1.0 mmole) of the product of Example 279, 0.5 ml (4.8 mmol) of diethylamine and 0.172 ml (2.0 mmol) of pyridine in 10 ml of dichloromethane was stired at room temperature for 18 hr. The resulting mixture washed with water and brine, dried over MgSO4, filtered and concentrated in vacuo. The residue was chromatographed on silica gel with 2% MeOH/CH2Cl2 as eluant to provide 425 mg (83%). Electrospray Mass Spec 511 (M+H).

후처리

  1. washThe resulting mixture washed with water and brine
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was chromatographed on silica gel with 2% MeOH/CH2Cl2 as eluant
  6. customto provide 425 mg (83%)

출처 및 근거

ORD 기록
ord-261f42fe32794305a58460d2bace5bae
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05929097

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