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Ammonium Chloride → HCID 14416771、化合物

HRID 1816945
ノート
印刷プレビュー

反応式

HRID 1816945 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 14416771HCID 14416771、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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))

出典と根拠

ORDレコード
ord-d771492979954edd8cb65726e067af1c
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07598244B2

反応ノート

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