反応式
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[N:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][C:12]=1[CH3:18])[CH3:9].[CH3:19][N:20]=[C:21]=[O:22]>C([O-])(=O)C.C([O-])(=O)C.C([Sn+2]CCCC)CCC.C(OCC)(=O)C>[CH3:19][NH:20][C:21](=[O:22])[O:17][C:14]1[CH:15]=[CH:16][C:11]([N:10]=[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[OH:1])[CH3:9])=[C:12]([CH3:18])[CH:13]=1参加物
実験手順
To a 350 milliliter glass pressure bottle equipped with a magnetic stirrer was added 4.83 grams (0.020 moles) of 4-[1-(2-hydroxyphenyl)ethylideneamino]-3-methylphenol prepared in Part A, 1.42 grams (0.025 moles) of methyl isocyanate, 100 milliliters of ethyl acetate and 5 drops of dibutyl tin diacetate. The resulting reaction mixture was stirred for 96 hours at room temperature, filtered and then washed twice with a 1% aqueous sodium bicarbonate solution followed by a single wash with saturated brine solution. After drying the reaction mixture over magnesium sulfate, it was concentrated under reduced pressure to give 5.36 grams (0.018 moles) of 4-[1-(2-hydroxyphenyl)ethylideneamino]-3-methylphenyl methylcarbamate in the form of an orange solid having a melting point of 133°-138° C. and the following structural formula: ##STR17##
後処理
- customThe resulting reaction mixture
- filtrationfiltered
- washwashed twice with a 1% aqueous sodium bicarbonate solution
- washa single wash with saturated brine solution
- dry with materialAfter drying the reaction mixture over magnesium sulfate, it
- concentrationwas concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-bd62958b724c4e23bfb4844405ab2ad8
- 出典データセット
- uspto-grants-1983_08
- 特許番号
- US04399148
関連ノート
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