Sodium Cyanide → HCID 86629102, 화합물

HRID 1097901노트

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HRID 1097901 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][C:13]=1[CH:14]([CH3:28])[C:15]([C:21]1[CH:26]=[CH:25][N:24]=[C:23]([Cl:27])[CH:22]=1)([OH:20])[C:16]([F:19])([F:18])[F:17])[CH2:5]OS(C)(=O)=O.[C-:29]#[N:30].[Na+]>CN(C=O)C.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:5][C:29]#[N:30])[CH:11]=[CH:12][C:13]=1[CH:14]([CH3:28])[C:15]([C:21]1[CH:26]=[CH:25][N:24]=[C:23]([Cl:27])[CH:22]=1)([OH:20])[C:16]([F:19])([F:18])[F:17]

참가 물질

5

반응물 2

HCID 8929Sodium CyanideHCID 86629101Methanesulfonic acid 3-chloro-4-[2-(2-chloro-pyridin-4-yl)-3,3,3-trifluoro-2-hydroxy-1-methyl-propyl]-benzyl ester

생성물 1

HCID 86629102HCID 86629102, 화합물수율 60.7%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
85 °C

실험 절차

Methanesulfonic acid 3-chloro-4-[2-(2-chloro-pyridin-4-yl)-3,3,3-trifluoro-2-hydroxy-1-methyl-propyl]-benzyl ester (66 mg) was dissolved in DMF at RT under argon. Sodium cyanide (18 mg) was added and the mixture was warmed to 85° C. and allowed to stir for 1.5 hours. The mixture was diluted with ethyl acetate and washed with water and brine. The organic extracts were dried over Na2SO4 and evaporated. The residue was purified by flash chromatography (silica gel, gradient of ethyl acetate in heptane) to give the desired compound as a colorless solid (34 mg). MS (m/e)=389.1 (MH+).

후처리

  1. washwashed with water and brine
  2. dry with materialThe organic extracts were dried over Na2SO4
  3. customevaporated
  4. customThe residue was purified by flash chromatography (silica gel, gradient of ethyl acetate in heptane)

출처 및 근거

ORD 기록
ord-2f2360c1d1084c3d8a8cf25d5d42992a
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143280B2

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