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Monobasic potassium phosphate → HCID 7091053, 화합물

HRID 339818
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HRID 339818 반응식
C([O:3][C:4](=[O:16])[CH2:5][CH:6]([NH2:15])[C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[F:14])C.P([O-])(O)(O)=O.[K+]>O>[NH2:15][C@H:6]([C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[F:14])[CH2:5][C:4]([OH:16])=[O:3]
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참가 물질

4

반응물 2

HCID 516951Monobasic potassium phosphateHCID 43312570Ethyl 3-amino-3-(2,5-difluorophenyl)propanoate

생성물 1

HCID 7091053HCID 7091053, 화합물수율 49.4%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

3-Amino-3-(2,5-difluorophenyl)propionic acid ethyl ester (3 g) was emulsified in water (pH=9.2) and admixed with potassium dihydrogenphosphate (5 mg) (pH=8.5). After addition of Amano Lipase PS (150 mg), the mixture was stirred overnight. The pH remains at 7.5. The mixture was then admixed with water (30 ml) and filtered through kieselguhr and washed several more times with water. The aqueous phase was then extracted with dichloromethane (3×30 ml), and the organic phase was dried (Na2SO4) and concentrated. This gave the product (1.3 g) with an ee=90% by HPLC.

후처리

  1. additionAfter addition of Amano Lipase PS (150 mg)
  2. filtrationfiltered through kieselguhr
  3. washwashed several more times with water
  4. extractionThe aqueous phase was then extracted with dichloromethane (3×30 ml)
  5. dry with materialthe organic phase was dried (Na2SO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-50215cbfa0844d518cd67d540ea07104
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08895547B2

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