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Imidazole → HCID 20565023, 화합물

HRID 225089
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HRID 225089 반응식
[CH2:1]([C:4]1([OH:10])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1)[C:2]#[CH:3].N1C=CN=[CH:12]1.Cl[SiH:17]([CH3:19])[CH3:18]>CN(C=O)C>[CH2:1]([C:4]1([O:10][Si:17]([CH3:19])([CH3:12])[CH3:18])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1)[C:2]#[CH:3]
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참가 물질

5

반응물 3

HCID 795ImidazoleHCID 66108ChlorodimethylsilaneHCID 879381-(2-Propynyl)cyclohexan-1-ol

생성물 1

HCID 20565023HCID 20565023, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of 55.4 g of 1-(2-propyn-1-yl)cyclohexanol [H. Gutmann, et al., Helv. Chim. Acta, 42, 719 (1959)] and 79 g of imidazole in 240 ml of DMF at 10° C. initially is added 56 ml of chlorodimethylsilane during 10 minutes. The cloudy yellow solution is stirred at room temperature for 26 hours. The resulting mixture is partitioned between 1000 ml of hexane and 400 ml of water at 0°-5° C. The hexane phase is washed successively with 6×200 ml of cold water and 200 ml of brine. The extract is dried over magnesium sulfate, filtered, and evaporated to give 85 g of colorless liquid, i.r. (film):1240 and 830 cm-1 (trimethylsilyloxy group).

후처리

  1. customThe resulting mixture is partitioned between 1000 ml of hexane and 400 ml of water at 0°-5° C
  2. washThe hexane phase is washed successively with 6×200 ml of cold water and 200 ml of brine
  3. dry with materialThe extract is dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-b22c577068104a51baaa120c388ee1d5
출처 데이터셋
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04235797

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