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Imidazole → Silane, (3-chloro-2,2-dimethylpropoxy)trimethyl-

HRID 36755
ノート
印刷プレビュー

反応式

HRID 36755 の反応式
[CH3:1][Si:2](Cl)([CH3:4])[CH3:3].N1C=CN=C1.[CH3:11][C:12]([CH3:17])([CH2:15][Cl:16])[CH2:13][OH:14]>C1CCCCC1>[CH3:1][Si:2]([CH3:4])([CH3:3])[O:14][CH2:13][C:12]([CH3:17])([CH3:11])[CH2:15][Cl:16]
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 795ImidazoleHCID 6397Chlorotrimethylsilane2 回HCID 834071-Propanol, 3-chloro-2,2-dimethyl-2 回

生成物 1

HCID 3018961Silane, (3-chloro-2,2-dimethylpropoxy)trimethyl-

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

実験手順

The initiator of structure (3), designated PFI10, was prepared using the procedures broadly described in WO 91 112277. The hydroxyl functionality in 2,2-dimethyl-3-chloropropanol was protected by reaction with trimethylsilyl chloride. A solution of trimethylsilyl chloride (27.16 g, 0.25 mol) in dry cyclohexane (150 g) was treated with 20.4 g of imidazole (0.30 mol) under an argon atmosphere. The resulting slurry was stirred vigorously at room temperature as 2,2-dimethyl-3-chloropropanol (30.93 g, 0.25 mol) was added slowly to the mixture. The rate of addition was controlled to keep the reaction temperature below 40° C. The resulting slurry was filtered affording a clear solution of the desired 1-trimethylsilyloxy-2,2-dimethyl-3-chloropropane. Analysis using a Gas Chromatography-Mass Spectroscopy (GC-MS) technique found essentially no side products. The trimethylsilyl protected adduct was obtained in quantitative yield. A repeat of this experiment gave similar results.

後処理

  1. customwas prepared
  2. additionwas added slowly to the mixture
  3. additionThe rate of addition
  4. customthe reaction temperature below 40° C
  5. filtrationThe resulting slurry was filtered

出典と根拠

ORDレコード
ord-378c79ed182d440eb6f83b18e5e65233
出典データセット
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05416168

反応ノート

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