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Methanol → HCID 23153952, 화합물

HRID 1175790
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HRID 1175790 반응식
[CH:1]([O:4][C:5]1[C:14]([O:15][CH3:16])=[CH:13][C:8]([C:9]([O:11]C)=[O:10])=[C:7]([NH:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=2)[CH:6]=1)([CH3:3])[CH3:2].CO.[OH-].[Na+]>O1CCCC1>[CH:1]([O:4][C:5]1[C:14]([O:15][CH3:16])=[CH:13][C:8]([C:9]([OH:11])=[O:10])=[C:7]([NH:17][CH2:18][C:19]2[CH:20]=[CH:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=2)[CH:6]=1)([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 23153963HCID 23153963, 화합물

생성물 1

HCID 23153952HCID 23153952, 화합물수율 99.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of methyl 4-isopropoxy-5-methoxy-2-(4-methoxybenzyl)aminobenzoate (18.9 g), methanol (50 ml), tetrahydrofuran (150 ml) and a 1N aqueous sodium hydroxide solution (80 ml) was stirred at room temperature for 1 night, heated under reflux for 12 hours. The solvent was distilled off under reduced pressure, the reaction mixture was adjusted to about pH 6 by adding 1N hydrochloric acid and 5% citric acid. The precipitated solid was collected by filtration, washed and dried to obtain the target compound (18.0 g).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 12 hours
  3. distillationThe solvent was distilled off under reduced pressure
  4. additionby adding 1N hydrochloric acid and 5% citric acid
  5. filtrationThe precipitated solid was collected by filtration
  6. washwashed
  7. customdried

출처 및 근거

ORD 기록
ord-be05615053164a6eadc4adca6121fe9d
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07842701B2

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