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Hydroxyphenylacetic acid → HCID 53677170, 화합물

HRID 1464626
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인쇄 미리보기

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HRID 1464626 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][CH:3]=1.[CH3:12][CH:13]1[CH2:18][C@H:17](O)[C@@H:16]([CH:20]([CH3:22])[CH3:21])[CH2:15][CH2:14]1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[OH:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([O:11][CH:15]2[CH:16]([CH:20]([CH3:22])[CH3:21])[CH2:17][CH2:18][CH:13]([CH3:12])[CH2:14]2)=[O:10])=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 127Hydroxyphenylacetic acidHCID 6101p-Toluenesulfonic acidHCID 12285346(+) Menthol

생성물 1

HCID 53677170HCID 53677170, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

2.9 kg of p-hydroxyphenylacetic acid and 1.95 kg of (+)-menthol are heated to boiling for 16 hours with 40 g of p-toluenesulphonic acid in 25 l of toluene; about 300 ml of water are separated in this process. The toluene solution is washed with 10 l of saturated NaHCO3 solution and 10 l of water and concentrated to dryness in vacuo. The title compound is obtained as 5.4 kg of oily residue (98-100% of theory) having a purity of 91.8% (HPLC surface area percentage). For analytical purposes, the (+)-menthylhydroxyphenylacetate was recrystallised twice from n-hexane.

후처리

  1. customabout 300 ml of water are separated in this process
  2. washThe toluene solution is washed with 10 l of saturated NaHCO3 solution and 10 l of water
  3. concentrationconcentrated to dryness in vacuo

출처 및 근거

ORD 기록
ord-a3371580324e4c62805ec8c83b39bf56
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05306820

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