Acetic Acid → HCID 21191979, compound

HRID 1457443Notes

Reaction equation

[OH:1][C:2]1[C:11]([C:12]([O:14][CH3:15])=[O:13])=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:16]([O:18][CH3:19])=[O:17])[CH:8]=2)[CH:3]=1.[C:20](O)(=[O:22])[CH3:21].CN(C)C=O.O>C(OC(=O)C)(=O)C.CN(C)C1C=CN=CC=1.CO>[C:20]([O:1][C:2]1[C:11]([C:12]([O:14][CH3:15])=[O:13])=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:16]([O:18][CH3:19])=[O:17])[CH:8]=2)[CH:3]=1)(=[O:22])[CH3:21]

Participants

Conditions

Temperature: 50 °C

Procedure

2-Hydroxy-3,6-di-methoxycarbonylnaphthalene (2.6 g) obtained in Example 26 was suspended in acetic anhydride (10.0 g), acetic acid (12.0 g) and N,N-dimethylformamide (20.0 g) and 4-dimethylaminopyridine (0.1 g) was added, followed by heating to 50° C. After heating for about 6 hours, the reaction solution was poured into a mixed solution of water (300 g) and methanol (100 g). The deposit was filtered and then washed with water to obtain 2.55 g of 2-acetoxy-3,6-di-methoxycarbonylnaphthalene as pale yellow powder (DSC analysis value: 130.6° C.).

Workup

temperatureAfter heating for about 6 hours
filtrationThe deposit was filtered
washwashed with water

Sources & evidence

ORD record: ord-0a7488ad63224bdb91a1c79f45743ae5
Source dataset: uspto-grants-1998_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05847233

Reaction notes

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