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Water → Methyl 6'-Desmethyl-4'-tosylmycophenolate

HRID 260107
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인쇄 미리보기

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HRID 260107 반응식
[OH:1][C:2]1[C:10]([CH3:11])=[C:9]2[C:5]([C:6](=[O:12])[O:7][CH2:8]2)=[C:4]([O:13][S:14]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)(=[O:16])=[O:15])[C:3]=1[CH2:24][CH:25]=[C:26]([CH3:32])[CH2:27][CH2:28][C:29]([OH:31])=[O:30].[C:33]1(C)C=CC(S(O)(=O)=O)=CC=1.O.C(OCC)(=O)C>CO>[OH:1][C:2]1[C:10]([CH3:11])=[C:9]2[C:5]([C:6](=[O:12])[O:7][CH2:8]2)=[C:4]([O:13][S:14]([C:17]2[CH:18]=[CH:19][C:20]([CH3:23])=[CH:21][CH:22]=2)(=[O:16])=[O:15])[C:3]=1[CH2:24]/[CH:25]=[C:26](\[CH3:32])/[CH2:27][CH2:28][C:29]([O:31][CH3:33])=[O:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 8857Ethyl AcetateHCID 536610776-(1,3-Dihydro-6-hydroxy-7-methyl-3-oxo-4-p-toluenesulfonyloxyisobenzofuran-5-yl)-4-methyl-4-hexenoic acid

생성물 1

HCID 10672181Methyl 6'-Desmethyl-4'-tosylmycophenolate

시약·촉매·용매 1

HCID 887
Methanol
용매

실험 절차

A solution of (E) 6-(1,3-dihydro-6-hydroxy-7-methyl-3-oxo-4-p-toluenesulfonyloxyisobenzofuran-5-yl)-4-methyl-4-hexenoic acid (23 g) and p-toluenesulfonic acid (0.8 g) in methanol (150 ml) was stirred for 18 hours then added to water and ethyl acetate. The organc layer was dried and evaporated and the residue was chromatographed on silica gel, eluting with hexane:ethyl acetate: methanol 40:58:2, to afford methyl (E) 6-(1,3-dihydro-6-hydroxy-7-methyl-3-oxo-4-p-toluenesulfonyloxyisobenzofuran-5-yl)-4-methyl-4-hexenoate.

후처리

  1. customThe organc layer was dried
  2. customevaporated
  3. customthe residue was chromatographed on silica gel
  4. washeluting with hexane:ethyl acetate: methanol 40:58:2

출처 및 근거

ORD 기록
ord-9abf809c48bd4787ad7365c82a2f4d53
출처 데이터셋
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05525602

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