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

HRID 1593920
ノート
印刷プレビュー

反応式

HRID 1593920 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

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

生成物 1

HCID 99422122-Hydroxy-2,2-dimethylethyl methacrylate

試薬・触媒・溶媒 3

HCID 21218Trioctylmethylammonium chloride触媒HCID 8008Butyronitrile溶媒
HCID 8058
Hexane
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-33caa6e1a30949528023136a2a513e01
出典データセット
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07300739B2

反応ノート

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