4,4'-Dimethoxybenzoin → 4,4'-Dimethoxybibenzyl

HRID 371687

反応式

HRID 371687 の反応式
[C:1]1([C:9]([CH:11]([C:13]2[CH:20]=[CH:19][C:16]([O:17][CH3:18])=[CH:15][CH:14]=2)O)=O)[CH:8]=[CH:7][C:4]([O:5][CH3:6])=[CH:3][CH:2]=1.[C]=O.[H][H]>O.O.O.O.C([O-])(=O)C.[Co+2].C([O-])(=O)C.C(O)CCC>[CH3:18][O:17][C:16]1[CH:15]=[CH:14][C:13]([CH2:11][CH2:9][C:1]2[CH:2]=[CH:3][C:4]([O:5][CH3:6])=[CH:7][CH:8]=2)=[CH:20][CH:19]=1

参加物

6

反応物 3

HCID 954154,4'-DimethoxybenzoinHCID 178418361HCID 178418361、化合物2 回HCID 178418416HCID 178418416、化合物2 回

生成物 1

HCID 742614,4'-Dimethoxybibenzyl収率 90%

試薬・触媒・溶媒 2

HCID 61372Cobalt(II) acetate tetrahydrate触媒HCID 2631-Butanol溶媒

反応条件

温度
200 °C

実験手順

The autoclave described in EXAMPLE 1 was employed. To this autoclave was charged 11.0 grams (0.040 mole) of anisoin, 2.0 grams (0.0080 mole) of cobalt(II) acetate tetrahydrate, and 70 milliliters of 1-butanol. The autoclave was thereafter charged to 1100 psig with carbon monoxide and heated, with stirring at 800 rpm, to 200° C. Hydrogen was then charged to the autoclave to a total pressure of 3800 psig for a hydrogen to carbon monoxide molar ratio of 2:1. The reaction was allowed to continue for a period of 1 hour, and thereafter cooled to about 70° C. Gas chromatographic analysis of the homogeneous product solution indicated a 90 percent yield of 1,2-bis(4-methoxyphenyl)ethane.

後処理

  1. temperatureheated
  2. temperaturecooled to about 70° C

出典と根拠

ORDレコード
ord-16479aea846949118a4c0403df24c0c7
出典データセット
uspto-grants-1978_05
特許番号
US04087463

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