Imidazole → HCID 178506949、化合物

HRID 878620ノート

反応式

HRID 878620 の反応式
[OH:1][CH2:2][CH2:3][CH2:4][C:5]([O:7][Li:8])=[O:6].N1C=CN=C1.[CH3:14][C:15]([Si:18](Cl)([CH3:20])[CH3:19])([CH3:17])[CH3:16].O>CN(C=O)C>[Si:18]([O:1][CH2:2][CH2:3][CH2:4][C:5]([O:7][Li:8])=[O:6])([C:15]([CH3:17])([CH3:16])[CH3:14])([CH3:20])[CH3:19]

参加物

6

反応物 4

HCID 795ImidazoleHCID 962WaterHCID 28928tert-Butyldimethylsilyl chlorideHCID 178506948HCID 178506948、化合物

生成物 1

HCID 178506949HCID 178506949、化合物収率 89%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a suspension of 4-hydroxybutanoyloxylithium (5.17 g, 41.03 mmol) and 1H-imidazole (4.19 g, 61.55 mmol) in DMF (20 mL) was added TBSCl (7.42 g, 49.04 mmol) in portions at r.t. The reaction mixture was then stirred overnight. The reaction solution was poured into water and extracted with ethyl acetate three times. The organic phase separated and washed with water twice, brine and dried with anhydrous Na2SO4. It was then concentrated to give the title compound as colorless oil (8.0 g, 89%). [M+H] Calc'd for C10H21LiO3Si, 225; Found, 225.

後処理

  1. extractionextracted with ethyl acetate three times
  2. customThe organic phase separated
  3. washwashed with water twice
  4. dry with materialbrine and dried with anhydrous Na2SO4
  5. concentrationIt was then concentrated

出典と根拠

ORDレコード
ord-19f41911f6094d9ea1bb4fedaf53aabf
出典データセット
uspto-grants-2015_03
特許番号
US08987461B2

反応ノート

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