Methanol → Tert-butyl 2-amino-4-(benzo[1,3]dioxol-5-yl)benzoate

HRID 1673359

반응식

HRID 1673359 반응식
CO.[O:3]1[C:7]2[CH:8]=[CH:9][C:10]([C:12]3[CH:24]=[CH:23][C:15]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])=[C:14]([N+:25]([O-])=O)[CH:13]=3)=[CH:11][C:6]=2[O:5][CH2:4]1>[C].[Pd].C(OCC)(=O)C>[NH2:25][C:14]1[CH:13]=[C:12]([C:10]2[CH:9]=[CH:8][C:7]3[O:3][CH2:4][O:5][C:6]=3[CH:11]=2)[CH:24]=[CH:23][C:15]=1[C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17]

참가 물질

5

반응물 2

HCID 887MethanolHCID 67342074Tert-butyl 4-(benzo[1,3]dioxol-5-yl)-2-nitrobenzoate

생성물 1

HCID 67342168Tert-butyl 2-amino-4-(benzo[1,3]dioxol-5-yl)benzoate

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 8857Ethyl Acetate용매

실험 절차

0.42 g of 10% palladium-carbon was added to a mixed solution of 14 mL of methanol and 14 mL of ethyl acetate containing 1.4 g of tert-butyl 4-(benzo[1,3]dioxol-5-yl)-2-nitrobenzoate and stirred under hydrogen atmosphere at room temperature for 2 hours. After insoluble were removed by filtration, the solvent was evaporated under reduced pressure. The obtained residue was purified with silica gel column chromatography [PSQ100B (spherical) manufactured by Fuji Silysia Chemical Ltd., eluent; hexane:ethyl acetate=20:1] to obtain 0.52 g of tert-butyl 2-amino-4-(benzo[1,3]dioxol-5-yl)benzoate as pale red solid.

후처리

  1. customAfter insoluble were removed by filtration
  2. customthe solvent was evaporated under reduced pressure
  3. customThe obtained residue was purified with silica gel column chromatography [PSQ100B (spherical) manufactured by Fuji Silysia Chemical Ltd., eluent; hexane:ethyl acetate=20:1]

출처 및 근거

ORD 기록
ord-21dfbbc2fa594164a90f99835772d944
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07999132B2

연결된 노트

불러오는 중…