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2-Iodophenol → HCID 58488432、化合物

HRID 1510071
ノート
印刷プレビュー

反応式

HRID 1510071 の反応式
[I:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8].[CH3:9][O:10][CH2:11][CH2:12][CH2:13]O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>C1COCC1>[I:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][CH2:13][CH2:12][CH2:11][O:10][CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 107842-IodophenolHCID 11776TriphenylphosphineHCID 741163-Methoxy-1-propanolHCID 75555Diisopropyl diazene-1,2-dicarboxylate

生成物 1

HCID 58488432HCID 58488432、化合物収率 100.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 2-iodophenol (3.00 g, 13.6 mmol), 3-methoxy-1-propanol (1.57 ml, 16.4 mmol) and triphenylphosphine (4.29 g, 16.4 mmol) in THF (15 ml) was added dropwise diisopropyl azodicarboxylate (3.22 ml, 16.4 mmol). The reaction mixture was stirred at room temperature overnight. The mixture was quenched with water and extracted with EA. The organic layer was separated, dried over sodium sulfate, filtered, and evaporated under reduced pressure: The residue was purified by silica gel chromatography (EA/HEP 1:5). 4.00 g of the title compound were obtained.

後処理

  1. customThe mixture was quenched with water
  2. extractionextracted with EA
  3. customThe organic layer was separated
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customThe residue was purified by silica gel chromatography (EA/HEP 1:5)

出典と根拠

ORDレコード
ord-3e4d96ad4df742d7bd64b58191e135b5
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08211885B2

反応ノート

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