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HCID 21075864, 화합물 → HCID 21075853, 화합물

HRID 1374160
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HRID 1374160 반응식
[Cl:1][C:2]1[C:3]([C:21]#[N:22])=[N:4][CH:5]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[C:9]=2[C:15]2[N:16]=[N:17][N:18]([CH3:20])[N:19]=2)[CH:7]=1>[NH4+].CO.[Ni]>[Cl:1][C:2]1[C:3]([CH2:21][NH2:22])=[N:4][CH:5]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[C:9]=2[C:15]2[N:16]=[N:17][N:18]([CH3:20])[N:19]=2)[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 21075864HCID 21075864, 화합물

생성물 1

HCID 21075853HCID 21075853, 화합물

시약·촉매·용매 3

HCID 935Nickel촉매HCID 223Ammonium용매HCID 887Methanol용매

실험 절차

To a solution of 3-chloro-5-[3-fluoro-2-(2-methyl-2H-tetrazol-5-yl)phenyl]-pyridine-2-carbonitrile (0.500 g, 1.59 mmol) in ammonium in methanol (40 mL 2.0 M) was added Raney 2800 nickel (slurry in water). The reaction mixture was stirred under H2 atmosphere for 3 hours, filtered through glass filter paper and concentrated under vacuum. The residue was azeotroped three times with toluene to yield crude 1-{3-chloro-5-[3-fluoro-2-(2-methyl-2H-tetrazol-5-yl)phenyl]pyridin-2-yl}methanamine that gave a mass ion (ES+) of 319.18 for M+H+.

후처리

  1. filtrationfiltered through glass
  2. filtrationfilter paper
  3. concentrationconcentrated under vacuum
  4. customThe residue was azeotroped three times with toluene

출처 및 근거

ORD 기록
ord-0256770ad27b4fff829e4543d32db34f
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07163951B2

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