Hydrochloric Acid → 1156914-56-5

HRID 2282345노트

반응식

HRID 2282345 반응식
[Br:1][C:2]1[CH:23]=[CH:22][C:5]([O:6][CH2:7][CH2:8][CH2:9][CH2:10][N:11]2C(=O)C3=CC=CC=C3C2=O)=[CH:4][CH:3]=1.O.NN.Cl>C(O)C.ClCCl>[Br:1][C:2]1[CH:23]=[CH:22][C:5]([O:6][CH2:7][CH2:8][CH2:9][CH2:10][NH2:11])=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 58473571HCID 58473571, 화합물

생성물 1

HCID 435310881156914-56-5수율 75%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6344Dichloromethane용매

반응 조건

온도
80 °C

실험 절차

N(4-(4-bromophenoxy)butyl)phthalimide (6.01 g, 16.1 mmol) is dissolved in ethanol (200 mL) under nitrogen, followed by the addition of hydrazine monohydrate (7.8 mL, 161 mmol). The reaction was refluxed at 80° C. for 2 hours. Once reaction completed (solids formed at the top layer), cooled reaction to room temperature and neutralized with 1M HCl (50 mL). The mixture is allowed to stir until all solids are completely dissolved and diluted with dichloromethane (150 mL). The solution was extracted with two portions of saturated NaHCO3 (2×). The organic layers were combined, washed with brine and water, then dried over MgSO4, and filtered. Removal of solvent yields a yellow oil (2.93 g, 75%).

후처리

  1. customOnce reaction
  2. customformed at the top layer),
  3. temperaturecooled
  4. customreaction to room temperature
  5. dissolutionare completely dissolved
  6. extractionThe solution was extracted with two portions of saturated NaHCO3 (2×)
  7. washwashed with brine and water
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customRemoval of solvent

출처 및 근거

ORD 기록
ord-5ed20ae4fc984445b028561fc89f9219
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09139869B2

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