Methyl iodide → HCID 13073255、化合物

HRID 67650ノート

反応式

HRID 67650 の反応式
[H-].[Na+].FC(F)(F)C1C=C(C2C(N)=C(C(OC)=O)SN=2)C=CC=1.CI.[CH3:25][NH:26][C:27]1[C:28]([C:36]2[CH:41]=[CH:40][CH:39]=[C:38]([C:42]([F:45])([F:44])[F:43])[CH:37]=2)=[N:29][S:30][C:31]=1[C:32]([O:34]C)=[O:33]>O1CCCC1>[F:45][C:42]([F:43])([F:44])[C:38]1[CH:37]=[C:36]([C:28]2[C:27]([NH:26][CH3:25])=[C:31]([C:32]([OH:34])=[O:33])[S:30][N:29]=2)[CH:41]=[CH:40][CH:39]=1

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 13073199Methyl 4-amino-3-[3-(trifluoromethyl)phenyl]-1,2-thiazole-5-carboxylateHCID 20265399HCID 20265399、化合物

生成物 1

HCID 13073255HCID 13073255、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of 0.5 g. of sodium hydride (washed free of mineral oil) in 15 ml. of tetrahydrofuran was cooled to -20° C. and stirred. To the cold stirred suspension was added in one portion 3.0 g. of methyl 3-(3-trifluoromethylphenyl)-4-amino-5-isothiazolecarboxylate. The reaction mixture was warmed to room temperature, at which time 1.5 ml. of methyl iodide was added in one portion. The reaction mixture was stirred at ambient temperature for two hours, and then was added to 50 ml. of ice water. The aqueous mixture was extracted several times with diethyl ether. The ethereal extracts were combined, washed with water, dried and the solvent was removed by evaporation under reduced pressure to afford 2.0 g. of methyl 4-methylamino-3-(3-trifluoromethylphenyl)-5-isothiazolecarboxylate.

後処理

  1. additionA suspension of 0.5 g
  2. stirringTo the cold stirred suspension
  3. additionwas added in one portion 3.0 g
  4. stirringThe reaction mixture was stirred at ambient temperature for two hours
  5. additionwas added to 50 ml
  6. extractionThe aqueous mixture was extracted several times with diethyl ether
  7. washwashed with water
  8. customdried
  9. customthe solvent was removed by evaporation under reduced pressure
  10. customto afford 2.0 g

出典と根拠

ORDレコード
ord-c0df6d52a0734ee18176b4e4379b42e5
出典データセット
uspto-grants-1982_08
特許番号
US04346094

反応ノート

読み込み中…