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

HRID 1612706ノート

反応式

HRID 1612706 の反応式
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]

参加物

3

反応物 2

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

生成物 1

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

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-fabb741967044524968f38e3208d24f6
出典データセット
uspto-grants-1993_03
特許番号
US05190933

反応ノート

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