Phthalaldehydic acid → (3-Oxo-1,3-dihydro-isobenzofuran-1-yl)-(2,4,4-trimethylpentyl)-phosphinic acid

HRID 1661855ノート

反応式

HRID 1661855 の反応式
[C:1]([C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH:6]=[O:7])([OH:3])=O.[CH3:12][CH:13]([CH2:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:14][PH:15](=[O:17])[OH:16]>C1(C)C(C)=CC=CC=1>[O:3]=[C:1]1[C:4]2[C:5](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]([P:15]([CH2:14][CH:13]([CH3:12])[CH2:18][C:19]([CH3:22])([CH3:21])[CH3:20])(=[O:16])[OH:17])[O:7]1

参加物

4

反応物 2

HCID 8406Phthalaldehydic acidHCID 178460681HCID 178460681、化合物

生成物 1

HCID 57909099(3-Oxo-1,3-dihydro-isobenzofuran-1-yl)-(2,4,4-trimethylpentyl)-phosphinic acid収率 56%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

A mixture of 15 grams (0.1 moles) of 2-carboxybenzaldehyde and 17.82 grams of 2,4,4-trimethylpentyl phosphinic acid in 100 mL of xylene is heated to reflux and 1.8 mL of water is collected by azeotropic distillation using a Dean-Stark receiver. The xylene solvent is removed in vacuo and the residue is crystallized with a mixture of 50 mL of ethyl acetate and 100 mL heptane to yield 17.2 grams (56% yield) (3-oxo-1,3-dihydro-isobenzofuran-1-yl)-(2,4,4-trimethylpentyl)-phosphinic acid as an off-white powder, mp 117-121° C.

後処理

  1. temperatureis heated
  2. temperatureto reflux
  3. distillation1.8 mL of water is collected by azeotropic distillation
  4. customThe xylene solvent is removed in vacuo
  5. customthe residue is crystallized with a mixture of 50 mL of ethyl acetate and 100 mL heptane

出典と根拠

ORDレコード
ord-03064dc1d79a41c499a68e3ad1a5145e
出典データセット
uspto-grants-2011_10
特許番号
US08030435B2

反応ノート

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