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Acetic Acid → 6,7-Dihydro-6-p-methoxybenzylthiO-5H-pyrrolo[2,1-c]-1,2,4-triazole

HRID 1089982
ノート
印刷プレビュー

反応式

HRID 1089982 の反応式
C(O[C:4]1[CH2:8][CH:7]([S:9][CH2:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)[CH2:6][N:5]=1)C.[CH:19]([NH:21][NH2:22])=O.C(O)(=O)C.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C.C(OCC)(=O)C>[CH3:18][O:17][C:14]1[CH:13]=[CH:12][C:11]([CH2:10][S:9][CH:7]2[CH2:6][N:5]3[C:4](=[N:22][N:21]=[CH:19]3)[CH2:8]2)=[CH:16][CH:15]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 10340Sodium CarbonateHCID 12229Hydrazinecarboxaldehyde2 回HCID 104680652-Ethoxy-4-p-methoxybenzylthio-1-pyroline

生成物 1

HCID 199785606,7-Dihydro-6-p-methoxybenzylthiO-5H-pyrrolo[2,1-c]-1,2,4-triazole

試薬・触媒・溶媒 2

HCID 702Ethanol
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

To a solution of 2-ethoxy-4-p-methoxybenzylthio-1-pyrroline (1.06 g) in ethanol (50 ml) there was added 0.36 g of formylhydrazine and heated to 80° C. under argon atmosphere while stirring. After 1.5 hours, 0.24 g of formylhydrazine was further added and stirred under heating for 30 minutes at the same temperature. Then, 0.6 g of acetic acid was added, stirred for 30 minutes at that temperature and then cooled to room temperature. To the cooled product were added ethyl acetate and 5% aqueous solution of sodium carbonate to distribute the product between these two liquids. The resulting organic phase was washed with saturated NaCl aqueous solution, dried over Na2SO4 and distilled off the solvent under reduced pressure to obtain the objective product.

後処理

  1. stirringstirred
  2. temperatureunder heating for 30 minutes at the same temperature
  3. stirringstirred for 30 minutes at that temperature
  4. temperaturecooled to room temperature
  5. washThe resulting organic phase was washed with saturated NaCl aqueous solution
  6. dry with materialdried over Na2SO4
  7. distillationdistilled off the solvent under reduced pressure
  8. customto obtain the objective product

出典と根拠

ORDレコード
ord-ac2b014234cc4c20a581363d77397680
出典データセット
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05079357

反応ノート

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