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

HRID 1673359

反応式

HRID 1673359 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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]

出典と根拠

ORDレコード
ord-21dfbbc2fa594164a90f99835772d944
出典データセット
uspto-grants-2011_08
特許番号
US07999132B2

関連ノート

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