Potassium Carbonate → 1,1,1-Triphenyl-1-sila-2-butene-4-ol

HRID 725201

반응식

HRID 725201 반응식
[C:1]1([Si:7]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:8]=[CH:9][CH2:10][O:11]C(=O)C)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)([O-])[O-].[K+].[K+]>CO>[C:1]1([Si:7]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:8]=[CH:9][CH2:10][OH:11])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 538005221,1,1-Triphenyl-4-acetoxy-1-sila-2-butene

생성물 1

HCID 543215981,1,1-Triphenyl-1-sila-2-butene-4-ol

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The crude acetoxy compound from Example 14 is dissolved in 250 mL methanol, and 25.0 g of potassium carbonate is added all at once. After stirring for 2 hours, the reaction mixture is filtered and concentrated. The concentrated residue is partitioned between 200/200 mL water/ethyl acetate. The organic layer is removed, washed with brine, dried and concentrated. The crude material is purified by flash chromatography using silica gel to afford the pure product.

후처리

  1. filtrationthe reaction mixture is filtered
  2. concentrationconcentrated
  3. customThe concentrated residue is partitioned between 200/200 mL water/ethyl acetate
  4. customThe organic layer is removed
  5. washwashed with brine
  6. customdried
  7. concentrationconcentrated
  8. customThe crude material is purified by flash chromatography
  9. customto afford the pure product

출처 및 근거

ORD 기록
ord-485864dcbf434954873bba8d9b687ce6
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705621

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