Hydrochloric Acid → HCID 178521618, 화합물

HRID 254415노트

반응식

HRID 254415 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:11][C:10](=[O:12])[CH2:9]2)=[CH:4][CH:3]=1.O.[Cl-].[NH4+].Cl>C1COCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C@@H:8]2[CH2:9][C@H:10]([OH:12])[CH2:11]2)=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 45896953-(4-Bromophenyl)cyclobutan-1-oneHCID 57429219Ammonium chloride monohydrate

생성물 1

HCID 178521618HCID 178521618, 화합물수율 66.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

At −78° C., 1.0 M tri(tert-butoxy)lithiumaluminium hydride (24 mL, 24 mmol) was added to a THF (20 mL) solution of 3-(4-bromophenyl)cyclobutanone (4.53 g, 20.1 mmol), and stirred at the same temperature for 1.5 hours. Saturated ammonium chloride water and 1 N hydrochloric acid were added to the reaction liquid, extracted with ethyl acetate, dried with anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure, the obtained residue was purified by silica gel column chromatography (C-200, ethyl acetate:hexane=1:4 to 3:7) to obtain the entitled compound (3.04 g, 66%).

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialdried with anhydrous magnesium sulfate
  3. concentrationThe solvent was concentrated under reduced pressure
  4. customthe obtained residue was purified by silica gel column chromatography (C-200, ethyl acetate:hexane=1:4 to 3:7)

출처 및 근거

ORD 기록
ord-ffd1d72c1d7a4c14a619a620f99ba6ee
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875633B2

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