Triethylamine → HCID 21890853、化合物

HRID 721463ノート

反応式

HRID 721463 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:22]=[CH:21][C:19]([NH2:20])=[C:18]([CH3:23])[C:17]=1[CH3:24].C([N:27](CC)CC)C.[C:32](Cl)(Cl)=[S:33].[CH2:36]([N:40]([CH2:45][CH2:46][CH2:47][CH3:48])[CH2:41][CH:42](N)[CH3:43])[CH2:37][CH2:38][CH3:39]>CN(C)C=O.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:22]=[CH:21][C:19]([NH:20][C:32]([NH:27][CH2:43][CH2:42][CH2:41][N:40]([CH2:36][CH2:37][CH2:38][CH3:39])[CH2:45][CH2:46][CH2:47][CH3:48])=[S:33])=[C:18]([CH3:23])[C:17]=1[CH3:24]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 10040ThiophosgeneHCID 21394028N~1~,N~1~-Dibutylpropane-1,2-diamineHCID 218904394-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylaniline

生成物 1

HCID 21890853HCID 21890853、化合物収率 37%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

4-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylaniline (51 mg) was dissolved in N,N-dimethylformamide (2 ml) and triethylamine (1 ml) to prepare a solution. Thiophosgene (51 mg) was then added to the solution, and the mixture was stirred at room temperature for 6 hr. Next, N,N-dibutylpropylenediamine (50 mg) was added thereto, and the mixture was further stirred at room temperature for 15 hr. Ethyl acetate was added to the reaction solution, followed by washing with water and saturated brine in that order. The organic layer was then dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by HPLC using chloroform/methanol for development to give the title compound (33 mg, yield 37%).

後処理

  1. stirringthe mixture was further stirred at room temperature for 15 hr
  2. washby washing with water and saturated brine in that order
  3. dry with materialThe organic layer was then dried over anhydrous sodium sulfate
  4. customThe solvent was removed by distillation under the reduced pressure
  5. customthe residue was purified by HPLC

出典と根拠

ORDレコード
ord-d569792d33d848ee94793bf64836cc47
出典データセット
uspto-grants-2006_11
特許番号
US07135466B2

反応ノート

読み込み中…