2-Acetylamino-5-(4,5-dihydro-furan-2-yl)-4-trifluoromethyl-benzoic acid methyl ester → 2-Acetylamino-5-(tetrahydro-furan-2-yl)-4-trifluoromethyl-benzoic acid methyl ester

HRID 1441554ノート

反応式

HRID 1441554 の反応式
[CH3:1][O:2][C:3](=[O:23])[C:4]1[CH:9]=[C:8]([C:10]2[O:11][CH2:12][CH2:13][CH:14]=2)[C:7]([C:15]([F:18])([F:17])[F:16])=[CH:6][C:5]=1[NH:19][C:20](=[O:22])[CH3:21]>C1COCC1.[Ni]>[CH3:1][O:2][C:3](=[O:23])[C:4]1[CH:9]=[C:8]([CH:10]2[CH2:14][CH2:13][CH2:12][O:11]2)[C:7]([C:15]([F:17])([F:18])[F:16])=[CH:6][C:5]=1[NH:19][C:20](=[O:22])[CH3:21]

参加物

4

反応物 1

HCID 585329042-Acetylamino-5-(4,5-dihydro-furan-2-yl)-4-trifluoromethyl-benzoic acid methyl ester

生成物 1

HCID 585329182-Acetylamino-5-(tetrahydro-furan-2-yl)-4-trifluoromethyl-benzoic acid methyl ester収率 100%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 2-acetylamino-5-(4,5-dihydro-furan-2-yl)-4-trifluoromethyl-benzoic acid methyl ester (13.2 g, 40.1 mmol) in dry THF (250 mL) was shaken under H2 (5 bars) at r.t. in the presence of Raney nickel. (6.0 g, B113W, Degussa) for 46 h. The reaction mixture was then filtered through a sintered funnel and the filtrate was concentrated in vacuo to give the title product (7.5 g, 100%) as a yellow oil. API-ES: m/z 332 [M+H]+.

後処理

  1. filtrationThe reaction mixture was then filtered through a sintered funnel
  2. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-df264dd7a01443bd8a8c9bc2fb56f914
出典データセット
uspto-grants-2010_02
特許番号
US07655666B2

反応ノート

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