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2,6-Dihydroxyanthraquinone → HCID 53655413、化合物

HRID 1600473
ノート
印刷プレビュー

反応式

HRID 1600473 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 53655413HCID 53655413、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ad4abfbcf9ae429c9f79a37c477e5d63
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05976486

反応ノート

読み込み中…

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