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

HRID 274707노트

반응식

HRID 274707 반응식
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

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 24654Hydrazine hydrate (1:1)HCID 14538888HCID 14538888, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e058e9d332854dbe8f4961e693e9f2c3
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05389658

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