Water → HCID 69522199、化合物

HRID 1181429

反応式

HRID 1181429 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 69522199HCID 69522199、化合物収率 19.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-414e8a5c44594230bd4f03687af284a8
出典データセット
uspto-grants-2007_10
特許番号
US07285563B2

関連ノート

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