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Hydrochloric Acid → Ethyl (3-aminobutyl)(diethoxymethyl)phosphinate

HRID 1612688
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HRID 1612688 반응식
O=[C:2]([CH3:17])[CH2:3][CH2:4][P:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])(=[O:9])[O:6][CH2:7][CH3:8].C([O-])(=O)C.[NH4+].C([BH3-])#[N:24].[Na+].Cl>CO>[NH2:24][CH:2]([CH3:17])[CH2:3][CH2:4][P:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])(=[O:9])[O:6][CH2:7][CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 14362820Ethyl 3-oxobutyl(diethoxymethyl)phosphinate

생성물 1

HCID 14362822Ethyl (3-aminobutyl)(diethoxymethyl)phosphinate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 1.0 g of ethyl 3-oxobutyl(diethoxymethyl)phosphinate 2.85 g of ammonium acetate and 0.16 g of sodium cyanoborohydride in 20 ml of methanol is stirred for 2.5 hours. After standing overnight, the pH is adjusted to pH 5,6 with 2N hydrochloric acid. The mixture is then evaporated to dryness. 20 ml of water are added and the mixture is washed 3 times with 20 ml of diethyl ether. The aqueous layer is adjusted to pH 12 with potassium hydroxide and extracted 4 times with 25 ml of chloroform. The organic layers are combined, dried, filtered and evaporated to dryness yielding ethyl 3-aminobutyl(diethoxymethyl)phosphinate, 31P-NMR spectrum: δ=+46.0 ppm (CDCl3).

후처리

  1. waitAfter standing overnight
  2. customThe mixture is then evaporated to dryness
  3. addition20 ml of water are added
  4. washthe mixture is washed 3 times with 20 ml of diethyl ether
  5. extractionextracted 4 times with 25 ml of chloroform
  6. customdried
  7. filtrationfiltered
  8. customevaporated to dryness

출처 및 근거

ORD 기록
ord-77030fa7adb54b28a3a50773edbf272f
출처 데이터셋
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05190933

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