Imidazole → 3-Triethylsilyloxy-1-octyne

HRID 224552

반응식

HRID 224552 반응식
[CH:1]#[C:2][CH:3]([OH:9])[CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].N1C=CN=C1.CN(C)C=O.Cl[Si:21]([CH2:26][CH3:27])([CH2:24][CH3:25])[CH2:22][CH3:23]>CCCCCC.O.C1C=CC=CC=1.C(OCC)(=O)C>[CH2:22]([Si:21]([CH2:26][CH3:27])([CH2:24][CH3:25])[O:9][CH:3]([CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[C:2]#[CH:1])[CH3:23]

참가 물질

8

반응물 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 131661-Octyn-3-olHCID 13819Chlorotriethylsilane

생성물 1

HCID 126753463-Triethylsilyloxy-1-octyne

시약·촉매·용매 3

HCID 241Benzene용매HCID 8857Ethyl Acetate용매HCID 22114717Water hexane용매

실험 절차

To a magnetically stirred solution of 50 g of 1-octyn-3-ol, 83 g of imidazole, and 500 ml of anhydrous dimethylformamide, cooled in an ice-water bath under an argon atmosphere, is slowly added 90 g of chlorotriethylsilane. After several minutes the reaction mixture is warmed to ambient temperature, and the progress of the reaction is monitored by tlc (1:4/ethyl acetate:benzene). On completion, the reaction mixture is poured into 500 ml of an iced mixture of 1:1 hexane-water. The organic phase is separated, washed with water and brine, dried over sodium sulfate and concentrated in vacuo. The resulting oil is distilled to provide 83 g (bp 70°-72° C., 0.35 mm).

후처리

  1. customThe organic phase is separated
  2. washwashed with water and brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. distillationThe resulting oil is distilled
  6. customto provide 83 g (bp 70°-72° C., 0.35 mm)

출처 및 근거

ORD 기록
ord-9524ce4d84364356a2c5d4e376b163b2
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04233231

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