2,2-Dimethyl-1,3-dioxane-4,6-dione → Methyl 4-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)-2-hydroxybenzoate

HRID 387913노트

반응식

HRID 387913 반응식
[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[CH2:6][C:4](=[O:5])[O:3]1.[CH:11](OCC)(OCC)OCC.[NH2:21][C:22]1[CH:31]=[CH:30][C:25]([C:26]([O:28][CH3:29])=[O:27])=[C:24]([OH:32])[CH:23]=1>CC(O)C>[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[C:6](=[CH:11][NH:21][C:22]2[CH:31]=[CH:30][C:25]([C:26]([O:28][CH3:29])=[O:27])=[C:24]([OH:32])[CH:23]=2)[C:4](=[O:5])[O:3]1

참가 물질

5

반응물 3

HCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 31214Ethyl orthoformateHCID 77787Methyl p-aminosalicylate

생성물 1

HCID 22936485Methyl 4-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)-2-hydroxybenzoate수율 95.8%

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
100 °C

실험 절차

After adding Meldrum acid (7.2 g, 50 mmol), triethyl orthoformate (50 ml) and 2-propanol (50 ml) to the publicly known compound methyl 4-amino-2-hydroxybenzoate (7.59 g, 45.4 mmol), the mixture was stirred at 100° C. for 1 hour. Upon cooling to room temperature, the precipitated crystals were filtered out, washed with diethyl ether and blow-dried to obtain the title compound (13.98 g, 43.5 mmol, 95.8%) as white crystals.

후처리

  1. temperatureUpon cooling to room temperature
  2. filtrationthe precipitated crystals were filtered out
  3. washwashed with diethyl ether
  4. customblow-dried

출처 및 근거

ORD 기록
ord-2a773fc96b5b4ace839134f9124fcd4e
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372981B2

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