Methyl 3,5-dichloro-4-hydroxybenzoate → 4,4'-[1,4-Phenylenebis([2,2-dimethyl-1,3-propanediyl]-oxycarbonyl)]bis(2,6-dichlorophenol)

HRID 971915

反応式

[OH:1][CH2:2][C:3]([CH3:18])([CH3:17])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12]([CH3:16])([CH3:15])[CH2:13][OH:14])=[CH:7][CH:6]=1.[Cl:19][C:20]1[CH:21]=[C:22]([CH:27]=[C:28]([Cl:31])[C:29]=1[OH:30])[C:23](OC)=[O:24]>C([O-])(=O)C.[Ca+2].C([O-])(=O)C.[Sb]=O>[C:8]1([CH2:11][C:12]([CH3:16])([CH3:15])[CH2:13][O:14][C:23]([C:22]2[CH:27]=[C:28]([Cl:31])[C:29]([OH:30])=[C:20]([Cl:19])[CH:21]=2)=[O:24])[CH:9]=[CH:10][C:5]([CH2:4][C:3]([CH3:18])([CH3:17])[CH2:2][O:1][C:23]([C:22]2[CH:27]=[C:28]([Cl:31])[C:29]([OH:30])=[C:20]([Cl:19])[CH:21]=2)=[O:24])=[CH:6][CH:7]=1

参加物

反応条件

温度: 200 °C

実験手順

A mechanically stirred mixture of 0.6 g of calcium acetate, 0.6 g of antimony oxide, 3.75 g (0.15 M) of 1,4-bis(3-hydroxy-2,2-dimethylpropyl)benzene and 132 g (0.6 M) of methyl 3,5-dichloro-4-hydroxybenzoate was heated under nitrogen atmosphere at 200° C. for 18 hours. The reaction mixture was washed three times with benzene in a Waring Blendor and extracted for 5 days with 2 liters of hot benzene. The extract, on cooling, yielded 70 g of 4,4'-[1,4-phenylenebis([2,2-dimethyl-1,3-propanediyl]oxycarbonyl)]bis(2,6-dichlorophenol) melting at 203°-204° C. The infrared spectrum was consistent with the indicated structure. The compound contained 3.185 meq. of OH/g indicating a molecular weight of 628 for the bisphenol.

後処理

washThe reaction mixture was washed three times with benzene in a Waring Blendor
extractionextracted for 5 days with 2 liters of hot benzene
temperatureThe extract, on cooling

出典と根拠

ORDレコード: ord-fd7265c52c7c44f48a36ca0ee8b655d8
出典データセット: uspto-grants-1979_07
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04161607

反応式

参加物

反応物 2

生成物 1

試薬・触媒・溶媒 2

反応条件

実験手順

後処理

出典と根拠

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