Ethyl Acetate → Methyl 2-amino-3-methoxybenzoate

HRID 576326

反応式

HRID 576326 の反応式
[CH3:1][O:2][C:3]1[C:4]([N+:13]([O-])=O)=[C:5]([CH:10]=[CH:11][CH:12]=1)[C:6]([O:8][CH3:9])=[O:7].CCOC(C)=O>C1COCC1.CO.[Pd]>[NH2:13][C:4]1[C:3]([O:2][CH3:1])=[CH:12][CH:11]=[CH:10][C:5]=1[C:6]([O:8][CH3:9])=[O:7]

参加物

6

反応物 2

HCID 8857Ethyl AcetateHCID 79195Benzoic acid, 3-methoxy-2-nitro-, methyl ester

生成物 1

HCID 602320Methyl 2-amino-3-methoxybenzoate収率 99.7%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of compound 52 (26.2 g, 124 mmol) and Pd/C (10 wt. %, 6.0 g) in THF (400 mL) and MeOH (200 mL) was stirred under an atmosphere of H2 at room temperature for 18 hours. EtOAc (300 mL) was added to the mixture and filtered through a Celite pad. The filtrate was concentrated in vacuo to provide the crude product 53 (22.4 g, 99%) as colorless oil.

後処理

  1. filtrationfiltered through a Celite pad
  2. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-08f1985b2e514371aac935c3e9cd63df
出典データセット
uspto-grants-2015_05
特許番号
US09034921B2

関連ノート

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