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 1894032ノート

反応式

HRID 1894032 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-a0d0be2767da43529f1869c94cbd10d2
出典データセット
uspto-grants-2013_08
特許番号
US08513268B2

反応ノート

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