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

HRID 1661855노트

반응식

HRID 1661855 반응식
[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

참가 물질

4

반응물 2

HCID 8406Phthalaldehydic acidHCID 178460681HCID 178460681, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-03064dc1d79a41c499a68e3ad1a5145e
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030435B2

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