Imidazole → HCID 11437113、化合物

HRID 549511

反応式

HRID 549511 の反応式
N1C=CN=C1.[CH2:6]=[CH:7][CH2:8][CH:9]([OH:13])[CH2:10][CH:11]=[CH2:12].[CH:14]([Si:17](Cl)([CH:21]([CH3:23])[CH3:22])[CH:18]([CH3:20])[CH3:19])([CH3:16])[CH3:15]>O>[CH:14]([Si:17]([CH:21]([CH3:23])[CH3:22])([CH:18]([CH3:20])[CH3:19])[O:13][CH:9]([CH2:10][CH:11]=[CH2:12])[CH2:8][CH:7]=[CH2:6])([CH3:16])[CH3:15]

参加物

5

反応物 3

HCID 795ImidazoleHCID 17902Hepta-1,6-dien-4-olHCID 139400Triisopropylsilyl chloride

生成物 1

HCID 11437113HCID 11437113、化合物収率 46%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

There was supplied 1.35 g of imidazole manufactured by Wako Pure Chemical Industries, Ltd. to a 50 mL-Schlenk tube, and thereto, 10 mL of anhydrous N,N-dimethylformaide manufactured by Wako Pure Chemical Industries, Ltd., and 1.2 mL of 1,6-heptadien-4-ol manufactured by Aldrich Chemical Company were added. The obtained mixture was cooled down to 0° C. To the mixture, 1.93 mL of triisopropylsilyl chloride manufactured by Tokyo Chemical Industry Co., Ltd. was added, and the resultant mixture was stirred for 85 hours at a room temperature. Then, an excess amount of water was added thereto, thereby terminating the reaction. A product contained in the reaction mixture was extracted with hexane, and the obtained organic extract was dried over anhydrous sodium sulfate manufactured by Nacalai Tesque, Inc. The dried hexane solution was distilled in vacuo, thereby obtaining 1.1 g (yield: 46%) of 4-(triisopropylsiloxy)-1,6-heptadiene at 93° C. under 21 mmHg as clear colorless oil.

後処理

  1. additionwere added
  2. additionwas added
  3. customterminating
  4. customthe reaction
  5. extractionwas extracted with hexane
  6. extractionthe obtained organic extract
  7. dry with materialwas dried over anhydrous sodium sulfate
  8. distillationThe dried hexane solution was distilled in vacuo

出典と根拠

ORDレコード
ord-858f803cdc954b77844d9d005ce30940
出典データセット
uspto-grants-2011_05
特許番号
US07943715B2

関連ノート

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