Triethylamine → HCID 9956174, 화합물

HRID 1740806

반응식

HRID 1740806 반응식
[CH3:1][S:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[C:12]([F:15])([F:14])[F:13])[N:8]([C:16](=[O:27])[NH:17][C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([OH:26])=O)[CH:19]=1)[CH2:7][CH2:6]2.C(Cl)(=O)C(Cl)=O.[CH3:34][N:35]([CH3:39])[CH2:36][CH2:37][NH2:38].C(N(CC)CC)C.[OH-].[Na+]>ClCCl.CN(C)C=O.O1CCCC1.O>[CH3:1][S:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[C:12]([F:15])([F:14])[F:13])[N:8]([C:16](=[O:27])[NH:17][C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([C:24](=[O:26])[NH:38][CH2:37][CH2:36][N:35]([CH3:39])[CH3:34])[CH:19]=1)[CH2:7][CH2:6]2

참가 물질

10

반응물 5

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 65578Oxalyl chlorideHCID 66053N,N-DimethylethylenediamineHCID 180051075-Methylthio-6-trifluoromethyl-1-(3-carboxy Phenyl Carbamoyl)indoline

생성물 1

HCID 9956174HCID 9956174, 화합물수율 45%

시약·촉매·용매 4

HCID 6228Dimethylformamide촉매HCID 962Water용매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of 5-methylthio-6-trifluoromethyl-1-(3-carboxy phenyl carbamoyl) indoline (0.5 g, 1.26mmol) in dichloromethane (20 ml) was added oxalyl chloride (0.3 ml, 2.52 mmol) and dimethylformamide (3 drops). After effervescing had subsided the reaction mixture was evaporated to dryness under reduced pressure. It was then dissolved in tetrahydrofuran (30 ml) and added to a solution of N,N-dimethylethylenediamine (0.405 g, 6.33mmol) and triethylamine (0.2 ml, 1.4 mmol) in tetrahydrofuran at 0° C. After 2 hours the reaction mixture was basified with 5M NaOH and water was added forming a white precipitate. This was filtered and dried to give the product a white solid (0.25 g, 45%), m.p. 91-93° C.

후처리

  1. customwas evaporated to dryness under reduced pressure
  2. dissolutionIt was then dissolved in tetrahydrofuran (30 ml)
  3. additionwas added
  4. customforming a white precipitate
  5. filtrationThis was filtered
  6. customdried

출처 및 근거

ORD 기록
ord-f8280e4dd96b47f9a1c79f68bf4aa884
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05972937

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