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Ammonium Chloride → HCID 14416771, 화합물

HRID 1816945
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HRID 1816945 반응식
[CH3:1][C:2]1([CH2:7][CH2:8][C:9](=[O:11])[CH3:10])[O:6][CH2:5][CH2:4][O:3]1.[CH3:12][Mg]Br.[Cl-].[NH4+]>O1CCCC1>[CH3:10][C:9]([OH:11])([CH2:8][CH2:7][C:2]1([CH3:1])[O:3][CH2:4][CH2:5][O:6]1)[CH3:12]
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참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 5383774-(2-Methyl-1,3-dioxolan-2-yl)-2-butanoneHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 14416771HCID 14416771, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The obtained 4-(2-methyl[1,3]dioxolan-2-yl)butan-2-one (27.60 g) was dissolved in tetrahydrofuran (220 ml), and thereafter, methylmagnesium bromide (3 M tetrahydrofuran solution; 85 ml) was added to the solution at a room temperature. The obtained mixture was stirred for 40 minutes, and an aqueous saturated ammonium chloride solution (300 ml) was then added thereto, followed by extraction with ethyl acetate (300 ml×3). The organic layer was washed with a saturated saline solution, and then dried over anhydrous sodium sulfate. The solvent was then distilled off under a reduced pressure. The residue was purified by silica gel column chromatography (eluted with ethyl acetate-hexane (1:1)) to obtain 2-methyl-4-(2-methyl[1,3]dioxolan-2-yl)butan-2-ol (21.18 g).

후처리

  1. extractionfollowed by extraction with ethyl acetate (300 ml×3)
  2. washThe organic layer was washed with a saturated saline solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was then distilled off under a reduced pressure
  5. customThe residue was purified by silica gel column chromatography (eluted with ethyl acetate-hexane (1:1))

출처 및 근거

ORD 기록
ord-d771492979954edd8cb65726e067af1c
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07598244B2

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