Dimethyl 5-aminoisophthalate → 5-amino-N,N'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-1,3-benzenedicarboxamide

HRID 1296196ノート

反応式

HRID 1296196 の反応式
[NH2:1][CH:2]([CH2:5][OH:6])[CH2:3][OH:4].[CH3:7][O-:8].[Na+].CO[C:12]([C:14]1[CH:19]=[C:18]([NH2:20])[CH:17]=[C:16]([C:21]([O:23]C)=O)[CH:15]=1)=[O:13]>CO>[NH2:20][C:18]1[CH:19]=[C:14]([C:12]([NH:1][CH:2]([CH2:3][OH:4])[CH2:7][OH:8])=[O:13])[CH:15]=[C:16]([C:21]([NH:1][CH:2]([CH2:5][OH:6])[CH2:3][OH:4])=[O:23])[CH:17]=1

参加物

5

反応物 3

HCID 66831Dimethyl 5-aminoisophthalateHCID 68294SerinolHCID 10942334Sodium Methoxide

生成物 1

HCID 99452455-amino-N,N'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-1,3-benzenedicarboxamide収率 93%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

2-Amino-1,3-dihydroxypropane (27.4 g, 300 mmol) and 1.5M solution of sodium methylate in methanol (14.3 mL, 21.5 mmol) are added to a suspension of 5-amino-1,3-benzenedicarboxylic acid dimethyl ester (30.0 g, 143 mmol) in methanol (0.2 L). The reaction mixture is heated to the reflux temperature to get a solution. After 2.5 hours of reflux and 4 hours at room temperature the reaction mixture is filtered and the solid on filter is washed with methanol (40 mL) and dried yielding the product of the title (43.5 g, 133 mmol, yield: 93%).

後処理

  1. temperatureThe reaction mixture is heated to the reflux temperature
  2. customto get a solution
  3. filtrationis filtered
  4. filtrationthe solid on filter
  5. washis washed with methanol (40 mL)
  6. customdried
  7. customyielding the product of the title (43.5 g, 133 mmol, yield: 93%)

出典と根拠

ORDレコード
ord-5a1341bed4614c468d89a9aaf9bf12f3
出典データセット
uspto-grants-2007_07
特許番号
US07244864B2

反応ノート

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