Ethyl Acetate → 4-[(Pyridin-4-yl)sulfanyl]butan-1-amine

HRID 6164ノート

反応式

HRID 6164 の反応式
C1(=O)[N:5]([CH2:6][CH2:7][CH2:8][CH2:9][S:10][C:11]2[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=2)C(=O)C2=CC=CC=C12.O.NN.C(OCC)(=O)C>C(O)C>[NH2:5][CH2:6][CH2:7][CH2:8][CH2:9][S:10][C:11]1[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 24654Hydrazine hydrate (1:1)HCID 14538888HCID 14538888、化合物

生成物 1

HCID 135575374-[(Pyridin-4-yl)sulfanyl]butan-1-amine収率 100.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of 12.50 g (40 mmol) of 4-(4-phthalimidobutylthio)pyridine in 200 ml of ethanol, 5.82 ml (120 mmol) of hydrazine monohydrate was added, and the mixture was stirred at room temperature for 4 hours. Then, 200 ml of ethyl acetate was-added, and the insoluble material was filtered off. The volatile components were distilled off and chloroform was added to the residue. The mixture was washed with saturated saline and dried over potassium carbonate. The solvent was distilled off and 7.30 g of the desired compound were obtained (quantitative yield, yellow oil).

後処理

  1. additionwas added
  2. filtrationthe insoluble material was filtered off
  3. distillationThe volatile components were distilled off
  4. additionchloroform was added to the residue
  5. washThe mixture was washed with saturated saline
  6. dry with materialdried over potassium carbonate
  7. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-eada9dfe6c2247098ac3fc6740df3411
出典データセット
uspto-grants-1993_09
特許番号
US05246948

反応ノート

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