Methyl iodide → HCID 13457751, 화합물

HRID 280125노트

반응식

HRID 280125 반응식
[Cl:1][C:2]1[CH:20]=[CH:19][CH:18]=[CH:17][C:3]=1[C:4]([C:6]1[N:7]([NH:11][C:12](=[O:16])[O:13][CH2:14][CH3:15])[CH:8]=[CH:9][CH:10]=1)=[O:5].[C:21](=O)([O-])[O-].[Na+].[Na+].CI>CN(C=O)C>[Cl:1][C:2]1[CH:20]=[CH:19][CH:18]=[CH:17][C:3]=1[C:4]([C:6]1[N:7]([N:11]([CH3:21])[C:12](=[O:16])[O:13][CH2:14][CH3:15])[CH:8]=[CH:9][CH:10]=1)=[O:5]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10340Sodium CarbonateHCID 13457750HCID 13457750, 화합물

생성물 1

HCID 13457751HCID 13457751, 화합물수율 65.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

[2-(2-Chlorobenzoyl)-1H-pyrrol-1-yl]-carbamic acid, ethyl ester (22 g, 75.1 mmol), sodium carbonate (16.0 g, 0.112 mol) and methyl iodide (13 g, 0.122 mol) were added to 100 ml of dry DMF and the mixture stirred at ambient temperature for 78 hours. The reaction was quenched with 1 liter of H2O and extracted with five 200 ml portions of diethyl ether. The combined extracts were washed with water and brine, dried (MgSO4), filtered, and evaporated to give 15 g of solid. This solid was purified by HPLC (silica gel, DCM) to give 13.1 g (57%) of crystals, m.p. 54°-56°.

후처리

  1. customThe reaction was quenched with 1 liter of H2O
  2. extractionextracted with five 200 ml portions of diethyl ether
  3. washThe combined extracts were washed with water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-63071b00f20f475e8ee901ff7381bf22
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04588727

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