tert-Butanol → HCID 66816641, 화합물

HRID 1755073

반응식

HRID 1755073 반응식
[C:1]([OH:5])([CH3:4])([CH3:3])[CH3:2].CCN=C=NCCCN(C)C.[Br:17][C:18]1[C:26]([CH3:27])=[CH:25][C:21]([C:22](O)=[O:23])=[CH:20][C:19]=1[CH3:28]>CN(C)C1C=CN=CC=1.ClCCl>[C:1]([O:5][C:22](=[O:23])[C:21]1[CH:25]=[C:26]([CH3:27])[C:18]([Br:17])=[C:19]([CH3:28])[CH:20]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 3

HCID 6386tert-ButanolHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 179371424-Bromo-3,5-dimethylbenzoic acid

생성물 1

HCID 66816641HCID 66816641, 화합물수율 70%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매2회

실험 절차

Dehydrated tert-butanol (0.19 ml, 2.0 mmol), 4-dimethylaminopyridine (81 mg, 0.67 mmol) and EDCI (255 mg, 1.33 mmol) were added to a solution of 4-bromo-3,5-dimethyl-benzoic acid (123 mg, 0.535 mmol) in dichloromethane (1.0 ml) at 0° C., and the mixture was stirred at room temperature for 25 hours. The reaction mixture was diluted with dichloromethane, and the organic layer was washed with water, dried over MgSO4 and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=100/1→50/1) to give 4-bromo-3,5-dimethyl-benzoic acid tert-butyl ester (106 mg, 70%).

후처리

  1. washthe organic layer was washed with water
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=100/1→50/1)

출처 및 근거

ORD 기록
ord-fa5c856f9a334d85926eeed27de47450
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169254B2

연결된 노트

불러오는 중…