Water → HCID 69522199, 화합물

HRID 1181429

반응식

HRID 1181429 반응식
[C:1](=O)([O-])[O-].[K+].[K+].[N+:7]([C:10]1[CH:19]=[CH:18][CH:17]=[C:16]2[C:11]=1[CH:12]=[CH:13][N:14]=[C:15]2[C:20]([OH:22])=[O:21])([O-:9])=[O:8].IC.O>CN(C)C=O>[N+:7]([C:10]1[CH:19]=[CH:18][CH:17]=[C:16]2[C:11]=1[CH:12]=[CH:13][N:14]=[C:15]2[C:20]([O:22][CH3:1])=[O:21])([O-:9])=[O:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 2856465-Nitroisoquinoline-1-carboxylic acid

생성물 1

HCID 69522199HCID 69522199, 화합물수율 19.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Potassium carbonate (23 g, 167 mmol) was added to a solution of 5-nitro-isoquinoline-1-carboxylic acid (Description 104, 2.7 g, 12.4 mmol) in N,N-dimethylformamide (50 ml) at room temperature. Iodomethane (1.0 ml, 16.1 mmol) was then added and the reaction stirred at room temperature for 20 h. Water (300 ml) was added and the mixture was extracted with ethyl acetate (2×200 ml). The combined organic phases were washed with water (2×100 ml), brine (100 ml) then dried (Na2SO4) and evaporated. Purification of the residue by column chromatography eluting with ethyl acetate-isohexane (7:13 increasing to 1:1) gave the title compound (558 mg, 19%).

후처리

  1. extractionthe mixture was extracted with ethyl acetate (2×200 ml)
  2. washThe combined organic phases were washed with water (2×100 ml), brine (100 ml)
  3. dry with materialthen dried (Na2SO4)
  4. customevaporated
  5. customPurification of the residue by column chromatography
  6. washeluting with ethyl acetate-isohexane (7:13 increasing to 1:1)

출처 및 근거

ORD 기록
ord-414e8a5c44594230bd4f03687af284a8
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285563B2

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