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

HRID 1481542노트

반응식

HRID 1481542 반응식
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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d4f5219ee4d3421fb34338f6ae814dc6
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409915B2

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