Imidazole → HCID 67346559、化合物

HRID 1518247ノート

反応式

HRID 1518247 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[CH2:10][OH:11].N1C=CN=C1.[CH:17]([Si:20](Cl)([CH:24]([CH3:26])[CH3:25])[CH:21]([CH3:23])[CH3:22])([CH3:19])[CH3:18]>CN(C=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[CH2:10][O:11][Si:20]([CH:24]([CH3:26])[CH3:25])([CH:21]([CH3:23])[CH3:22])[CH:17]([CH3:19])[CH3:18]

参加物

5

反応物 3

HCID 795ImidazoleHCID 139400Triisopropylsilyl chlorideHCID 10867706(2-Bromo-5-methoxyphenyl)methanol

生成物 1

HCID 67346559HCID 67346559、化合物収率 94%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

(2-Bromo-5-methoxyphenyl)methanol (1 eq.) was dissolved in anhydrous DMF (1.1M solution) and imidazole (1.05 eq.) was added. To the stirred solution triisopropylsilyl chloride (1.1 eq.) was added and the resulting mixture was left stirring at RT for 8 h. All volatiles were evaporated in vacuo and the residual material was filtered with PE/EtOAc (9:1) over a pad of silica gel. After evaporation in vacuo the product was obtained as a colorless oil (94%), which was used without further characterization in the next reaction.

後処理

  1. waitthe resulting mixture was left
  2. customAll volatiles were evaporated in vacuo
  3. filtrationthe residual material was filtered with PE/EtOAc (9:1) over a pad of silica gel
  4. customAfter evaporation in vacuo the product

出典と根拠

ORDレコード
ord-46649b618eff41dc8a2be2d8f73d2e6b
出典データセット
uspto-grants-2012_07
特許番号
US08232390B2

反応ノート

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