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

HRID 964137ノート

反応式

HRID 964137 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-7a0b6c4ebc1741088b8a834b235c4c5a
出典データセット
uspto-grants-1998_06
特許番号
US05767121

反応ノート

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