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Hexane → Ethyl 2,6-dichloro-3-triisopropylsilyloxybenzoate

HRID 1604533
ノート
印刷プレビュー

反応式

HRID 1604533 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][Si:9]([CH:16]([CH3:18])[CH3:17])([CH:13]([CH3:15])[CH3:14])[CH:10]([CH3:12])[CH3:11])=[C:4]([Cl:19])[CH:3]=1.C([Li])CCC.CCCCCC.Cl[C:32]([O:34][CH2:35][CH3:36])=[O:33]>O1CCCC1>[Cl:19][C:4]1[C:5]([O:8][Si:9]([CH:13]([CH3:15])[CH3:14])([CH:16]([CH3:18])[CH3:17])[CH:10]([CH3:11])[CH3:12])=[CH:6][CH:7]=[C:2]([Cl:1])[C:3]=1[C:32]([O:34][CH2:35][CH3:36])=[O:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8058HexaneHCID 10928Ethyl chloroformateHCID 19603523HCID 19603523、化合物HCID 178418339Butyllithium

生成物 1

HCID 19603310Ethyl 2,6-dichloro-3-triisopropylsilyloxybenzoate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 1,3-dichloro-4-triisopropylsilyloxybenzene (6.00 g) in tetrahydrofuran (50 ml) at -60° C. was added dropwise n-butyllithium, 1.6M solution of hexane (12.9 ml) over 30 minutes under nitrogen and the mixture was stirred for 1 hour at the same temperature. A solution of ethyl chloroformate in tetrahydrofuran (20 ml) was added dropwise to the mixture over 20 minutes at -60° C. The resulting mixture is stirred for 1 hour at -60° C., the cooling bath was removed, and temperature was allowed to rise to 20° C. A solution of ammonium chloride (2 g) in water (37 ml) was then added over 5 minutes followed by ethyl acetate (40 ml) and brine (40 ml). The organic layer was separated, washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel eluting with a mixture of ethyl acetate and hexane (1:10 to 1:6) to give ethyl 2,6-dichloro-3-triisopropylsilyloxybenzoate (1.59 g) as an oil.

後処理

  1. stirringThe resulting mixture is stirred for 1 hour at -60° C.
  2. customthe cooling bath was removed
  3. customto rise to 20° C
  4. additionA solution of ammonium chloride (2 g) in water (37 ml) was then added over 5 minutes
  5. customThe organic layer was separated
  6. washwashed with water and brine
  7. dry with materialdried over magnesium sulfate
  8. customevaporated in vacuo
  9. customThe residue was chromatographed on silica gel eluting with a mixture of ethyl acetate and hexane (1:10 to 1:6)

出典と根拠

ORDレコード
ord-7f3af750ffaf4b54a7803eaba095b589
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05994368

反応ノート

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