Triethylamine → HCID 18707306, 화합물

HRID 1421980노트

반응식

HRID 1421980 반응식
[CH2:1]([N:3](CC)[CH2:4]C)C.[CH2:8]([O:10][C:11]1[CH:12]=[C:13]([C:20]2[S:21][CH:22]=[C:23]([C:25]3[N:30]=[C:29]([C:31](O)=[O:32])[CH:28]=[CH:27][CH:26]=3)[N:24]=2)[CH:14]=[CH:15][C:16]=1[O:17][CH2:18][CH3:19])[CH3:9].Cl.CNC.P(C#N)(OCC)(OCC)=O>CN(C)C=O.O>[CH2:8]([O:10][C:11]1[CH:12]=[C:13]([C:20]2[S:21][CH:22]=[C:23]([C:25]3[N:30]=[C:29]([C:31]([N:3]([CH3:4])[CH3:1])=[O:32])[CH:28]=[CH:27][CH:26]=3)[N:24]=2)[CH:14]=[CH:15][C:16]=1[O:17][CH2:18][CH3:19])[CH3:9]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 76257Diethyl cyanophosphonateHCID 3025803Tetomilast

생성물 1

HCID 18707306HCID 18707306, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

1.13 ml of triethylamine was dropwise added, at room temperature, to a solution of 1 g of 2-(3,4-diethoxyphenyl)-4-(2-carboxy-6-pyridyl)thiazole, 245 mg of dimethylamine hydrochloride and 515 mg of diethyl cyanophosphate in 15 ml of dimethylformamide. The mixture was stirred at the same temperature for 3 hours. The reaction mixture was mixed with 20 ml of water. The resulting mixture was extracted with 50 ml of dichloromethane three times. The dichloromethane layer was dried over sodium sulfate and concentrated. The residue was recrystallized from n-hexane-ethyl acetate-dichloromethane to obtain 800 mg of 2-(3,4-diethoxyphenyl)-4-(2-dimethylaminocarbonyl-6-pyridyl)thiazole.

후처리

  1. extractionThe resulting mixture was extracted with 50 ml of dichloromethane three times
  2. dry with materialThe dichloromethane layer was dried over sodium sulfate
  3. concentrationconcentrated
  4. customThe residue was recrystallized from n-hexane-ethyl acetate-dichloromethane

출처 및 근거

ORD 기록
ord-9cbd79285beb4a8eb83aa72c9ada2bde
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080764

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