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Potassium Hydroxide → HCID 19613993、化合物

HRID 1600474
ノート
印刷プレビュー

反応式

HRID 1600474 の反応式
[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]
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 14797Potassium HydroxideHCID 935522,6-DihydroxynaphthaleneHCID 14411016Diethyl (4-bromobutyl)phosphonate

生成物 1

HCID 19613993HCID 19613993、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e044e952609c43eab740f079d6d0c8e9
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

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