Sodium Hydroxide → 5-Ethynylpyridin-2-amine

HRID 558644노트

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HRID 558644 반응식
FC(F)(F)C1[N:8]2N=CC=[C:7]2[N:6]=[C:5]([C:12]2[CH:17]=[CH:16]C(C(F)(F)F)=[CH:14][CH:13]=2)C=1.[OH-].[Na+]>C1(C)C=CC=CC=1>[C:17]([C:12]1[CH:13]=[CH:14][C:7]([NH2:8])=[N:6][CH:5]=1)#[CH:16]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 715397317-(Trifluoromethyl)-5-(4-(trifluoromethyl)phenyl)pyrazolo[1,5-a]pyrimidine

생성물 1

HCID 219548275-Ethynylpyridin-2-amine수율 36.4%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 4-(6-amino-pyridin-3-yl)-2-methyl-but-3-yn-2-ol (example D.1 method 2 step 1) (22.5 g, 128 mmol) in toluene (500 mL) was refluxed in the presence of powdered NaOH (3.83 g, 96 mmol) for 16 h. The solvent was removed under reduced pressure to leave a brown residue which was purified by silica gel column chromatography with dichloromethane and ether, followed by trituration with heptane to give the title compound (5.5 g, 36%) (31.1 g, 100%) as light red solid. MS (EI) 118.1 [(M)+]; mp 143° C.

후처리

  1. customThe solvent was removed under reduced pressure
  2. customto leave a brown residue which
  3. customwas purified by silica gel column chromatography with dichloromethane and ether

출처 및 근거

ORD 기록
ord-f74fb5a3a3db47e19a5d10d7082cc796
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063048B2

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