Hydrochloric Acid → 3-Amino-2-hydroxy-propyl(ethyl)phosphinic acid hydrochloride

HRID 973633노트

반응식

HRID 973633 반응식
C1(=O)[N:5]([CH2:6][CH:7]([O:16][Si](C)(C)C)[CH2:8][P:9]([CH2:14][CH3:15])(=[O:13])[O:10]CC)C(=O)C2=CC=CC=C12.[ClH:27]>>[ClH:27].[NH2:5][CH2:6][CH:7]([OH:16])[CH2:8][P:9]([CH2:14][CH3:15])(=[O:10])[OH:13]

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 19090885Ethyl 3-phthalimido-2-trimethylsilyloxy-propyl(ethyl)phosphinate

생성물 1

HCID 856311253-Amino-2-hydroxy-propyl(ethyl)phosphinic acid hydrochloride

실험 절차

A solution of 6.4 g of ethyl 3-phthalimido-2-trimethylsilyloxy-propyl(ethyl)phosphinate in 100 ml of concentrated aqueous hydrochloric acid is heated to reflux for 20 hours. After this time the suspension is cooled to room temperature and filtered. The filtrate is evaporated to dryness, the resulting semi-solid is co-evaporated with water (5×50 ml) and absolute ethanol (5×100 ml) and the white solid is dried in high vacuum overnight. Crystallisation from absolute ethanol/acetone affords 3-amino-2-hydroxy-propyl(ethyl)phosphinic acid hydrochloride, m.p. 114°-115°.

후처리

  1. temperatureto reflux for 20 hours
  2. filtrationfiltered
  3. customThe filtrate is evaporated to dryness
  4. customthe white solid is dried in high vacuum overnight
  5. customCrystallisation from absolute ethanol/acetone

출처 및 근거

ORD 기록
ord-38fd71ecc3a849d6b5412c1cf1ee6d67
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05064819

반응 노트

불러오는 중…