Hydrochloric Acid → HCID 178521618、化合物

HRID 254415ノート

反応式

HRID 254415 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178521618HCID 178521618、化合物収率 66.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-ffd1d72c1d7a4c14a619a620f99ba6ee
出典データセット
uspto-grants-2011_01
特許番号
US07875633B2

反応ノート

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