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2,6-Dihydroxyanthraquinone → HCID 53655413, 화합물

HRID 1600473
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HRID 1600473 반응식
[OH:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12](=[O:16])[C:11]3[C:6](=[CH:7][CH:8]=[C:9]([OH:17])[CH:10]=3)[C:5](=[O:18])[C:4]=2[CH:3]=1.C([O:21][P:22]([CH2:27][CH2:28][CH2:29][CH2:30]Br)(=[O:26])[O:23]CC)C.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[P:22]([CH2:27][CH2:28][CH2:29][CH2:30][O:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12](=[O:16])[C:11]3[C:6](=[CH:7][CH:8]=[C:9]([O:17][CH2:30][CH2:29][CH2:28][CH2:27][P:22]([OH:21])([OH:23])=[O:26])[CH:10]=3)[C:5](=[O:18])[C:4]=2[CH:3]=1)([OH:26])([OH:23])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 67762,6-DihydroxyanthraquinoneHCID 11430Potassium CarbonateHCID 14411016Diethyl (4-bromobutyl)phosphonate

생성물 1

HCID 53655413HCID 53655413, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2,6-dihydroxyanthraquinone (1.19 g, 4.98 mmol) and diethyl(4-bromobutyl)phosphonate (3.0 g, 10 mmol) were heated at 60 ° C. in 5 ml DMF in the presence of 0.8 g of K2CO3 for 72 hours. The solution was extracted with CH2Cl2. The CH2Cl2 solution was dried, leaving a yellow 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. extractionThe solution was extracted with CH2Cl2
  2. dry with materialThe CH2Cl2 solution was dried
  3. customleaving a yellow solid
  4. customThe ester was purified by column chromatography
  5. additionfollowed by addition of water
  6. washThe bisphosphonic acid derivative was washed with CH2Cl2
  7. filtrationfiltered
  8. customcollected

출처 및 근거

ORD 기록
ord-ad4abfbcf9ae429c9f79a37c477e5d63
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05976486

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