Potassium Carbonate → HCID 69313855, 화합물

HRID 131187

반응식

HRID 131187 반응식
CS(O[C@H:6]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C@H:7]1[O:12][CH2:11][CH2:10][N:9]([C@@H:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH3:14])[CH2:8]1)(=O)=O.C(=O)([O-])[O-].[K+].[K+].[F:33][C:34]([F:43])([F:42])[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[SH:41]>>[C:15]1([C@H:13]([N:9]2[CH2:10][CH2:11][O:12][C@H:7]([C@H:6]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[S:41][C:36]3[CH:37]=[CH:38][CH:39]=[CH:40][C:35]=3[C:34]([F:33])([F:42])[F:43])[CH2:8]2)[CH3:14])[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

참가 물질

4

반응물 3

HCID 11430Potassium CarbonateHCID 27778892-(Trifluoromethyl)benzenethiolHCID 59732174HCID 59732174, 화합물

생성물 1

HCID 69313855HCID 69313855, 화합물수율 71%

실험 절차

A mixture of 51 (0.035 g, 0.093 mmol), potassium carbonate (0.026 g, 0.19 mmol) and 2-trifluoromethylbenzenethiol (0.084 g, 0.47 mmol) in dry, degassed dimethylformamide (0.5 ml) was stirred under nitrogen at room temperature for 3 days. The reaction mixture was diluted with water and extracted with diethyl ether. The extracts was washed with water and brine, dried over magnesium sulphate, filtered and evaporated to give a colourless oil (0.03 g, 71%). Purification by flash column chromatography (eluent: ethyl acetate/heptane 20/80 [v/v]) gave 52 as a colourless oil (0.03 g, 71%); MW 457.56; C26H26F3NOS 1H NMR (CDCl3) 7.53 (1H, d), 7.10-7.28 (13H, m), 4.39 (1H, d), 3.85-4.04 (2H, m), 3.8 (1H, td), 3.35 (1H, q), 2.70 (1H, d), 2.40 (1H, d), 2.30 (1H, td), 2.10-2.20 (1H, m), 1.29 (3H, d). m/z [M+H]+ 458.

후처리

  1. customin dry
  2. customdegassed dimethylformamide (0.5 ml)
  3. additionThe reaction mixture was diluted with water
  4. extractionextracted with diethyl ether
  5. washThe extracts was washed with water and brine
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-5515106e8c7d43c79231da658baddb5e
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07384941B2

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