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Sodium Hydroxide → HCID 178525066, 화합물

HRID 1489787
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HRID 1489787 반응식
C[O:2][PH:3]([CH2:5][CH:6]([CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:7]([O:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:8])=[O:4].[OH-].[Na+]>CO.O>[OH:4][PH:3]([CH2:5][CH:6]([CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:7]([O:9][CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)=[O:8])=[O:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 178502927HCID 178502927, 화합물

생성물 1

HCID 178525066HCID 178525066, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
0 °C

실험 절차

A solution of benzyl 2-((methoxyphosphinyl)methyl)-4-phenylbutanoate (4.02 g, 11.6 mmol) in methanol (20 mL) was cooled in an ice bath and 2.5N aqueous sodium hydroxide (5.1 mL. 12.8 mmol) was added over 10 min. The resulting solution was stirred at 0° C. for 45 min before being diluted with water (150 mL) and washed with a mixture of ether (75 mL) and hexane (25 mL). The aqueous layer was washed with hexane (75 mL), acidified by the addition of 2N aqueous hydrochloric acid (20 mL), and extracted with ethyl acetate (2×75 mL). The ethyl acetate layers were washed in succession with saturated aqueous sodium chloride (50 mL), dried (sodium sulfate), decanted, and evaporated. The residue was dried overnight under vacuum to give crude (±)-benzyl 2-((hydroxyphosphinyl)methyl)-4-phenylbutanoate as 3.67 g of colorless oil (95% yield).

후처리

  1. washwashed with a mixture of ether (75 mL) and hexane (25 mL)
  2. washThe aqueous layer was washed with hexane (75 mL)
  3. additionacidified by the addition of 2N aqueous hydrochloric acid (20 mL)
  4. extractionextracted with ethyl acetate (2×75 mL)
  5. washThe ethyl acetate layers were washed in succession with saturated aqueous sodium chloride (50 mL)
  6. dry with materialdried (sodium sulfate)
  7. customdecanted
  8. customevaporated
  9. customThe residue was dried overnight under vacuum

출처 및 근거

ORD 기록
ord-e2ee4a0a8f334660a4f63bce14118e94
출처 데이터셋
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05679700

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