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Potassium Hydroxide → HCID 19613993, 화합물

HRID 1600474
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HRID 1600474 반응식
[OH-:1].[K+].[OH:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[C:9]([OH:14])[CH:10]=2)[CH:5]=1.C([O:17][P:18]([CH2:23][CH2:24][CH2:25][CH2:26]Br)(=[O:22])[O:19]CC)C>C(O)C>[P:18]([CH2:23][CH2:24][CH2:25][CH2:26][O:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:14][CH2:26][CH2:25][CH2:24][CH2:23][P:18]([OH:17])([OH:19])=[O:22])[CH:10]=2)[CH:5]=1)([OH:19])([OH:17])=[O:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 935522,6-DihydroxynaphthaleneHCID 14411016Diethyl (4-bromobutyl)phosphonate

생성물 1

HCID 19613993HCID 19613993, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

1.34 g of KOH in ethanol were added dropwise to a mixture of 2,6-dihydroxynaphthalene (1.6g, 10 mmol) and diethyl(4-bromobutyl)phosphonate (6.0 g, 22 mmol) in ethanol, the mixture was left at room temperature for over night. The product was extracted with CH2Cl2. The CH2Cl2 solution was dried, leaving a brownish solid. The ester was purified by column chromatography. The bisphosphonate ester was converted to the acid by overnight stirring with 4-fold excess of bromotrimethylsilane in dry dichloromethane followed by addition of water. The bisphosphonic acid derivative was washed with CH2Cl2, filtered and collected.

후처리

  1. waitthe mixture was left at room temperature for over night
  2. extractionThe product was extracted with CH2Cl2
  3. dry with materialThe CH2Cl2 solution was dried
  4. customleaving a brownish solid
  5. customThe ester was purified by column chromatography
  6. additionfollowed by addition of water
  7. washThe bisphosphonic acid derivative was washed with CH2Cl2
  8. filtrationfiltered
  9. customcollected

출처 및 근거

ORD 기록
ord-e044e952609c43eab740f079d6d0c8e9
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05976486

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