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Hydrochloric Acid → P-(3-amino-1-hydroxy-propyl)-P-methyl-phosphinic acid hydrochloride

HRID 1198818
ノート
印刷プレビュー

反応式

HRID 1198818 の反応式
C(OC([NH:11][CH2:12][CH2:13][CH:14]([P:16]([CH3:21])(=[O:20])[O:17]CC)[OH:15])=O)C1C=CC=CC=1.[ClH:22]>>[ClH:22].[NH2:11][CH2:12][CH2:13][CH:14]([P:16]([CH3:21])(=[O:17])[OH:20])[OH:15]
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 2

HCID 313Hydrochloric AcidHCID 10403409ethyl P-(3-benzyloxycarbonylamino-1-hydroxy-propyl)-P-methyl-phosphinate

生成物 1

HCID 86747538P-(3-amino-1-hydroxy-propyl)-P-methyl-phosphinic acid hydrochloride

実験手順

A solution of 4.0 g of ethyl P-(3-benzyloxycarbonylamino-1-hydroxy-propyl)-P-methyl-phosphinate in 50 ml of 5.0M aqueous hydrochloric acid is heated to reflux for 20 hours under an inert gas atmosphere. Then, the reaction mixture is cooled to room temperature and washed twice with 100 ml each of dichloromethane and once with diethyl ether. The aqueous layer is evaporated to dryness at 50° under reduced pressure. The oily residue is then co-evaporated 5 times with 50 ml each of water and of absolute ethanol. The remaining white solid is dried under reduced pressure at 80° and then re-crystallised to afford P-(3-amino-1-hydroxy-propyl)-P-methyl-phosphinic acid hydrochloride of m.p. 115°-116.5°. This can be converted into the free compound by dissolving in ethanol and treating with propylene oxide yielding, after filtration and drying, P-(3-amino-1-hydroxy-propyl)-P-methyl-phosphinic acid of m.p. 125°-126.5°.

後処理

  1. temperatureto reflux for 20 hours under an inert gas atmosphere
  2. washwashed twice with 100 ml each of dichloromethane and once with diethyl ether
  3. customThe aqueous layer is evaporated to dryness at 50° under reduced pressure
  4. customThe remaining white solid is dried under reduced pressure at 80°
  5. customre-crystallised

出典と根拠

ORDレコード
ord-efb7353651314c9db3079dfccf5d1e1a
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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