(4-Methoxy-benzyl)-[4-trifluoromethyl-6-(2-trifluoromethyl-phenyl)-pyridin-2-yl]amine → 4-Trifluoromethyl-6-(2-trifluoromethyl-phenyl)-pyridin-2-ylamine

HRID 570222ノート

反応式

HRID 570222 の反応式
COC1C=CC(C[NH:8][C:9]2[CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=[C:11]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25]([F:28])([F:27])[F:26])[N:10]=2)=CC=1>CO.[Pd]>[F:18][C:15]([F:16])([F:17])[C:13]1[CH:12]=[C:11]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[C:25]([F:26])([F:28])[F:27])[N:10]=[C:9]([NH2:8])[CH:14]=1

参加物

4

反応物 1

HCID 86657408(4-Methoxy-benzyl)-[4-trifluoromethyl-6-(2-trifluoromethyl-phenyl)-pyridin-2-yl]amine

生成物 1

HCID 866574094-Trifluoromethyl-6-(2-trifluoromethyl-phenyl)-pyridin-2-ylamine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of (4-methoxy-benzyl)-[4-trifluoromethyl-6-(2-trifluoromethyl-phenyl)-pyridin-2-yl]-amine (1.00 g, 2.34 mmol, prepared as described in STEP B above) in MeOH (20 mL) was added, the flask was flushed well with Ar, Pd/C (500 mg, 0.235 mmol, 5% on carbon) was added, and the flask was flushed with Ar and fitted with an H2 balloon. The resulting mixture stirred at room temperature for 4 h. The balloon was removed, the flask was flushed again with Ar, the mixture was filtered through diatomaceous earth, and the filter cake was washed well with MeOH. The filtrate was concentrated in vacuo to yield 4-trifluoromethyl-6-(2-trifluoromethyl-phenyl)-pyridin-2-ylamine as a tan solid. 1H-NMR (400 MHz, CDCl3) δ: 7.81 (d, J=7.6 Hz, 1H), 7.64-7.76 (m, 2H), 7.59 (d, J=7.1 Hz, 1H), 7.25 (s, 1H), 6.79 (s, 1H), 3.22 (br. s., 4H).

後処理

  1. additionwas added
  2. customthe flask was flushed with Ar
  3. customfitted with an H2 balloon
  4. customThe balloon was removed
  5. customthe flask was flushed again with Ar
  6. filtrationthe mixture was filtered through diatomaceous earth
  7. washthe filter cake was washed well with MeOH
  8. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-05d2f8adf6b64496bc2fa722c3be2dd4
出典データセット
uspto-grants-2015_05
特許番号
US09023846B2

反応ノート

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