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

HRID 1296195노트

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HRID 1296195 반응식
CO[C:3]([C:5]1[CH:10]=[C:9]([NH2:11])[CH:8]=[C:7]([C:12]([O:14]C)=O)[CH:6]=1)=[O:4].[NH2:16][CH:17]([CH2:20][OH:21])[CH2:18][OH:19]>CO>[NH2:11][C:9]1[CH:10]=[C:5]([C:3]([NH:16][CH:17]([CH2:20][OH:21])[CH2:18][OH:19])=[O:4])[CH:6]=[C:7]([C:12]([NH:16][CH:17]([CH2:20][OH:21])[CH2:18][OH:19])=[O:14])[CH:8]=1

참가 물질

4

반응물 2

HCID 66831Dimethyl 5-aminoisophthalateHCID 68294Serinol

생성물 1

HCID 99452455-amino-N,N'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-1,3-benzenedicarboxamide수율 90%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
105 °C

실험 절차

5-Amino-1,3-benzenedicarboxylic acid dimethyl ester (40.0 g, 191 mmol) and 2-amino-1,3-dihydroxypropane (104.5 g, 1.147 mol) are loaded into a 1 L vessel equipped with a mechanical stirrer, a thermometer and a refluxing refrigerator. The suspension is heated up to 105° C., and is maintained at this temperature for 150 minutes to yield a solution. After cooling to 50° C., methanol (0.7 L) is added and the obtained suspension is maintained for 4 hours at room temperature. The solid that separates is filtered, washed with methanol (0.3 L), and dried in the oven at 45° C. for 4 hours yielding the compound of the title (56.3 g, 0.172 mol, yield: 90%).

후처리

  1. customequipped with a mechanical stirrer
  2. temperatureis maintained at this temperature for 150 minutes
  3. customto yield a solution
  4. temperatureAfter cooling to 50° C.
  5. temperaturethe obtained suspension is maintained for 4 hours at room temperature
  6. filtrationThe solid that separates is filtered
  7. washwashed with methanol (0.3 L)
  8. customdried in the oven at 45° C. for 4 hours
  9. customyielding the compound of the title (56.3 g, 0.172 mol, yield: 90%)

출처 및 근거

ORD 기록
ord-6abc1cb076a7426eaa6a68c2012b415d
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244864B2

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