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Phenothiazine → 2-Hydroxy-2,2-dimethylethyl methacrylate

HRID 1593920
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HRID 1593920 반응식
ClC[CH2:3][C:4]([CH3:7])([OH:6])[CH3:5].[C:8]([O-:13])(=[O:12])[C:9]([CH3:11])=[CH2:10].[Na+].C1C2NC3C(=CC=CC=3)SC=2C=CC=1>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].C(#N)CCC.CCCCCC>[C:8]([O:13][CH2:3][C:4]([OH:6])([CH3:7])[CH3:5])(=[O:12])[C:9]([CH3:11])=[CH2:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 7108PhenothiazineHCID 5477654-Chloro-2-methylbutan-2-olHCID 3255932Sodium methacrylate

생성물 1

HCID 99422122-Hydroxy-2,2-dimethylethyl methacrylate

시약·촉매·용매 3

HCID 21218Trioctylmethylammonium chloride촉매HCID 8008Butyronitrile용매
HCID 8058
Hexane
용매

실험 절차

A mixture of 1-chloromethyl-2-methyl-2-propanol (21.80 g, 0.20 mole), sodium methacrylate (32.40 g, 0.30 mole), Adogen 464 (7.00 g, 0.015 mole) (phase transfer catalyst purchased from Aldrich Chemical Co.), and phenothiazine (60 mg) in butyronitrile (200 ml) was heated to reflux under nitrogen in a three-necked round bottomed flask equipped with a condenser and a mechanical stirrer. After cooling the contents to room temperature, the mixture was diluted with hexane (200 ml) and filtered through celite. The solvents were removed under aspirator vacuum (40-80° C.). The residue was distilled under high vacuum. The 22.50 grams of the product was collected between 72-80° C. at 2 mm pressure as a clear liquid.

후처리

  1. temperaturewas heated
  2. temperatureto reflux under nitrogen in a three-necked round bottomed flask
  3. customequipped with a condenser and a mechanical stirrer
  4. filtrationfiltered through celite
  5. customThe solvents were removed under aspirator vacuum (40-80° C.)
  6. distillationThe residue was distilled under high vacuum
  7. customThe 22.50 grams of the product was collected between 72-80° C. at 2 mm pressure as a clear liquid

출처 및 근거

ORD 기록
ord-33caa6e1a30949528023136a2a513e01
출처 데이터셋
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07300739B2

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