Pyridine → HCID 11256949, 화합물

HRID 1602753노트

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HRID 1602753 반응식
[C:1](Cl)(=[O:5])[C:2]([CH3:4])=[CH2:3].[CH3:7][Si:8]([Si:11]([Si:19]([CH3:22])([CH3:21])[CH3:20])([Si:15]([CH3:18])([CH3:17])[CH3:16])[CH2:12][CH2:13][OH:14])([CH3:10])[CH3:9].N1C=CC=CC=1>O1CCCC1.C1C2NC3C(=CC=CC=3)SC=2C=CC=1>[C:1]([O:14][CH2:13][CH2:12][Si:11]([Si:19]([CH3:22])([CH3:21])[CH3:20])([Si:15]([CH3:18])([CH3:17])[CH3:16])[Si:8]([CH3:7])([CH3:9])[CH3:10])(=[O:5])[C:2]([CH3:4])=[CH2:3]

참가 물질

6

반응물 3

HCID 1049PyridineHCID 13528Methacryloyl chlorideHCID 133081222-[1,1,1,3,3,3-Hexamethyl-2-(trimethylsilyl)trisilan-2-yl]ethan-1-ol

생성물 1

HCID 11256949HCID 11256949, 화합물수율 63%

시약·촉매·용매 2

HCID 7108Phenothiazine촉매HCID 8028Tetrahydrofuran용매2회

실험 절차

Methacryloyl chloride (2.50 grams, 0.024 mole) in 25 ml tetrahydro-furan was added dropwise into a solution of 2-tris(trimethylsilyl) silyl ethanol (6.5 grams, 0.022 mole), pyridine (2.0 grams, 0.025 mole) and 25 mg of phenothiazine in 50 ml tetrahydrofuran at room temperature. Stirred at room temperature for two more hours. The solids were filtered off and the solution was washed with 100 ml brine. The solution was then diluted with 100 ml ether and washed with 5% hydrochloric acid, followed by deionzed water, and then with brine. It was dried over anhydrous magnesium sulfate and was concentrated in vacuo. Fractional distillation under reduced pressed gave 5 grams of the product at 105-115° C. at 0.5 mm.

후처리

  1. filtrationThe solids were filtered off
  2. washthe solution was washed with 100 ml brine
  3. additionThe solution was then diluted with 100 ml ether
  4. washwashed with 5% hydrochloric acid
  5. dry with materialIt was dried over anhydrous magnesium sulfate
  6. concentrationwas concentrated in vacuo
  7. distillationFractional distillation

출처 및 근거

ORD 기록
ord-66f14550627c402099b9e1e3563baa38
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05985524

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