Phosphoric Acid → 3-Cyclopentyl-1,1-dimethylpropyl acetate

HRID 2085010ノート

反応式

HRID 2085010 の反応式
[CH:1]1([CH2:6][CH2:7][C:8]([CH3:11])([OH:10])[CH3:9])[CH2:5][CH2:4][CH2:3][CH2:2]1.[C:12](OC(=O)C)(=[O:14])[CH3:13].OP(O)(O)=O>O>[C:12]([O:10][C:8]([CH3:11])([CH3:9])[CH2:7][CH2:6][CH:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1)(=[O:14])[CH3:13]

参加物

5

反応物 3

HCID 1004Phosphoric AcidHCID 7918Acetic AnhydrideHCID 22728826alpha,alpha-Dimethyl-cyclopentanepropanol

生成物 1

HCID 227288293-Cyclopentyl-1,1-dimethylpropyl acetate収率 100.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

10 g (64 mmol) of 4-cyclopentyl-2-methyl-2-butanol, 32.6 g (320 mmol) of acetic anhydride and a drop of H3PO4 (85% in water) were introduced in a 200 ml flask, and the mixture was stirred over night, at room temperature. Afterwards, 100 ml of water where added and the stirring was prolonged for an additional period of 2 hours. The crude product was extracted by washing the water solution with pentane. The organic phases thus obtained were washed twice with a saturated NaHCO3 water solution, then twice with brine and finally dried over MgSO4 and concentrated. It was thus obtained 12.7 g of crude product (quantitative yield) having a GC purity of 99%.

後処理

  1. extractionThe crude product was extracted
  2. washby washing the water solution with pentane
  3. customThe organic phases thus obtained
  4. washwere washed twice with a saturated NaHCO3 water solution
  5. dry with materialtwice with brine and finally dried over MgSO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-66a065b4c8c449a1862916b31e22eb40
出典データセット
uspto-grants-2004_04
特許番号
US06720295B2

反応ノート

読み込み中…