tert-Butanol → tert-Butyl 4-(methylamino)benzoate

HRID 446532노트

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HRID 446532 반응식
[CH3:1][NH:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([O-:9])=[O:8])=[CH:5][CH:4]=1.Cl.C(N=C=NCCCN(C)C)C.[C:24](O)([CH3:27])([CH3:26])[CH3:25]>CN(C)C1C=CN=CC=1>[CH3:1][NH:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([O:9][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:8])=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 6386tert-ButanolHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 69332534-(Methylamino)benzoate

생성물 1

HCID 22291264tert-Butyl 4-(methylamino)benzoate수율 78%

시약·촉매·용매 1

HCID 142844-(Dimethylamino)pyridine촉매

실험 절차

4-(Methylamino)benzoate (2.00 g, 13.2 mmol) was dissolved in tert-butanol (66 mL), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (89 mg, 0.464 mmol) and 4-dimethylaminopyridine (81 mg, 0.660 mmol) were added, and the mixture was stirred at room temperature for 17 hours. The solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=6:1, v/v) to give the title compound (2.14 g; yield, 78%) as a yellow oily substance.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. customthe resulting residue was purified by silica gel column chromatography (hexane

출처 및 근거

ORD 기록
ord-34e95d34a9ec49d99e6c07421a7ecd6a
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476253B2

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