Dichloromethane → [9H-Fluorene-9,9-diylbis(methyleneoxy)]bis(trimethylsilane)

HRID 2252528

반응식

HRID 2252528 반응식
[OH:1][CH2:2][C:3]1([CH2:16][OH:17])[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2.ClCCl.[CH3:21][Si:22](Cl)([CH3:24])[CH3:23]>C(N(CC)CC)C>[CH3:21][Si:22]([CH3:24])([CH3:23])[O:1][CH2:2][C:3]1([CH2:16][O:17][Si:22]([CH3:24])([CH3:23])[CH3:21])[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 6397ChlorotrimethylsilaneHCID 3450229H-Fluorene-9,9-dimethanol

생성물 1

HCID 22639095[9H-Fluorene-9,9-diylbis(methyleneoxy)]bis(trimethylsilane)수율 88%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

1 g of 9,9-bis(hydroxymethyl)-fluorene was admixed with 20 ml of dichloromethane. The mixture was cooled in ice-water bath, and 1.9 ml of triethyl amine was added thereto. Then 1.4 ml of trimethylsilyl chloride was added drop-wise, and the mixture was stirred in ice-water bath for further 2 hours. The reaction mixture was washed with water, and the organic layer separated was dried over anhydrous sodium sulfate. After filtration, the filtrate was evaporated to give 1.41 g of concentrate (yield 88%). The crude product was purified by column chromatography using petroleum ether as eluent, to give colorless pure compound. MS (El) m/e: 370(M+).

후처리

  1. washThe reaction mixture was washed with water
  2. customthe organic layer separated
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. filtrationAfter filtration
  5. customthe filtrate was evaporated
  6. customto give 1.41 g
  7. concentrationof concentrate (yield 88%)
  8. customThe crude product was purified by column chromatography
  9. customto give colorless pure compound

출처 및 근거

ORD 기록
ord-ec2192eefd9f4b1f82934f5e38b30b42
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07323431B2

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