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isobutyl P-(4-aminobut-2-yl)-P-methyl-phosphinate → (3-Amino-1-methyl-propyl)-methyl-phosphinic acid

HRID 1198808
ノート
印刷プレビュー

反応式

HRID 1198808 の反応式
[NH2:1][CH2:2][CH2:3][CH:4]([P:6]([CH3:13])(=[O:12])[O:7]CC(C)C)[CH3:5]>Cl>[NH2:1][CH2:2][CH2:3][CH:4]([P:6]([CH3:13])(=[O:7])[OH:12])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 23374771isobutyl P-(4-aminobut-2-yl)-P-methyl-phosphinate

生成物 1

HCID 10219532(3-Amino-1-methyl-propyl)-methyl-phosphinic acid

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of 21.5 g of isobutyl P-(4-aminobut-2-yl)-P-methyl-phosphinate in 80 ml of 36% aqueous hydrochloric acid is heated to reflux for a period of 10 hours. The reaction mixture is then allowed to cool to room temperature, concentrated under reduced pressure, and co-evaporated twice with 100 ml of water. The crude material is dissolved in water, washed with chloroform, and the aqueous layer treated with activated charcoal. The aqueous solution is filtered hot, evaporated to dryness, the crude product is dissolved in 50 ml of methanol and treated with 1-2 ml of propylene oxide. The hydroscopic solid is filtered and triturated with acetone. After drying, P-(4-aminobut-2-yl)-P-methyl-phosphinic acid is obtained as a hygroscopic solid, m.p. 68°-75°, 31P-NMR spectrum: δ=+46.5 ppm (D2O).

後処理

  1. temperatureto reflux for a period of 10 hours
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe crude material is dissolved in water
  4. washwashed with chloroform
  5. additionthe aqueous layer treated with activated charcoal
  6. filtrationThe aqueous solution is filtered hot
  7. customevaporated to dryness
  8. dissolutionthe crude product is dissolved in 50 ml of methanol
  9. additiontreated with 1-2 ml of propylene oxide
  10. filtrationThe hydroscopic solid is filtered
  11. customtriturated with acetone
  12. customAfter drying

出典と根拠

ORDレコード
ord-2670f3d068cb4812b00670278e35da2b
出典データセット
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05281747

反応ノート

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