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Phosphoric Acid → (2S,3S)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol phosphate

HRID 1992781
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HRID 1992781 반응식
[CH3:1][N:2]([CH3:18])[CH2:3][C@H:4]([CH3:17])[C@@:5]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([O:15][CH3:16])[CH:10]=1)([OH:8])[CH2:6][CH3:7].[P:19](=O)([OH:22])([OH:21])[OH:20]>C(O)C>[P:19]([O:8][C@@:5]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([O:15][CH3:16])[CH:10]=1)([CH2:6][CH3:7])[C@@H:4]([CH3:17])[CH2:3][N:2]([CH3:1])[CH3:18])([OH:22])([OH:21])=[O:20]
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참가 물질

4

반응물 2

HCID 1004Phosphoric AcidHCID 11708619(2S,3S)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol

생성물 1

HCID 68535694(2S,3S)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol phosphate수율 16%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

10 g (0.04 mol) of the enantiomeric pair (2R,3R)/(2S,3S)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol were dissolved in 40 ml of ethanol and treated with stirring with 3 g of 85 wt. % ortho-phosphoric acid. After 24 h, the crystals formed were filtered off under reduced pressure and dried for 24 h in a drying cabinet at 40° C. to a final pressure of 10 mbar. 2.2 g (16% of theoretical) of (2S,3S)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol phosphate were obtained as colourless crystals with an enantiomeric purity of 85%.

후처리

  1. additiontreated
  2. customthe crystals formed
  3. filtrationwere filtered off under reduced pressure
  4. customdried for 24 h in a drying cabinet at 40° C. to a final pressure of 10 mbar

출처 및 근거

ORD 기록
ord-5519e187898546dca10d6c4e36fc840b
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07649114B2

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