Methylamine → HCID 8180193、化合物

HRID 1782030

反応式

HRID 1782030 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[CH2:11][C:12]([OH:14])=O.C1N=C[N:17](C(N2C=NC=C2)=O)[CH:16]=1.CN.C(OCC)(=O)C>CN(C=O)C.O>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[CH2:11][C:12]([NH:17][CH3:16])=[O:14]

参加物

7

反応物 4

HCID 6329MethylamineHCID 8857Ethyl AcetateHCID 682631,1'-CarbonyldiimidazoleHCID 3505552-(2,4-Dimethoxyphenyl)acetic acid

生成物 1

HCID 8180193HCID 8180193、化合物収率 73.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of (2,4-dimethoxyphenyl)acetic acid (577 mg, 3.0 mmol) and N,N-carbonyldiimidazole (608 mg, 3.75 mmol) in DMF (10 mL) was stirred at room temperature for 45 min, aqueous 40% methyl amine (4.5 mL) was added and the reaction mixture was stirred at room temperature over the week-end. The reaction mixture was is partitoned between ethyl acetate and H2O. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel flash chromatography (0-80% ethyl acetate in petroleum spirit) to give the subtitled compound (460 mg).

後処理

  1. stirringthe reaction mixture was stirred at room temperature over the week-end
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel flash chromatography (0-80% ethyl acetate in petroleum spirit)

出典と根拠

ORDレコード
ord-ef69b6f7495e473da852aa96bc95b40c
出典データセット
uspto-grants-2009_03
特許番号
US07498338B2

関連ノート

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