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

HRID 1296196노트

반응식

HRID 1296196 반응식
[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

참가 물질

5

반응물 3

HCID 66831Dimethyl 5-aminoisophthalateHCID 68294SerinolHCID 10942334Sodium Methoxide

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-5a1341bed4614c468d89a9aaf9bf12f3
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244864B2

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