Water → HCID 69070098、化合物

HRID 2110016ノート

反応式

HRID 2110016 の反応式
[CH3:1][O:2][C:3](=[O:31])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])=[C:6]([NH:18][S:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[N+:28]([O-:30])=[O:29])(=[O:21])=[O:20])[CH:5]=1.[C:32](=O)([O-])[O-].[K+].[K+].CI.O>CN(C)C=O.C(OCC)(=O)C>[CH3:1][O:2][C:3](=[O:31])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([O:13][C:14]([CH3:17])([CH3:15])[CH3:16])=[O:12])=[C:6]([N:18]([CH3:32])[S:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[N+:28]([O-:30])=[O:29])(=[O:21])=[O:20])[CH:5]=1

参加物

7

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 69063936HCID 69063936、化合物

生成物 1

HCID 69070098HCID 69070098、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

After dissolving 4-tert-butoxycarbonylamino-3-(2-nitro-benzenesulfonylamino)-benzoic acid methyl ester (1.23 g, 2.73 mmol) in dimethylformamide (10 ml), potassium carbonate (1.13 g, 8.16 mmol) and methyl iodide (0.254 ml, 4.09 mmol) were added in an ice bath, and the mixture was stirred at room temperature for 2 hours. Water (100 ml) was added to the reaction mixture, and extraction was performed with ethyl acetate (40 ml×4 times). The obtained organic layer was washed with saturated brine and then dried over anhydrous magnesium sulfate. After concentration under reduced pressure, the crystallized residue was dried to obtain 4-tert-butoxycarbonylamino-3-[methyl-(2-nitro-benzenesulfonyl)-amino]-benzoic acid methyl ester. The compound was identified by LC-MS.

後処理

  1. additionwere added in an ice bath
  2. washThe obtained organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationAfter concentration under reduced pressure
  5. customthe crystallized residue was dried

出典と根拠

ORDレコード
ord-a877cb0a548e44e6bed30c3415bb7164
出典データセット
uspto-grants-2009_04
特許番号
US07517875B2

反応ノート

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