Dichloromethane → HCID 54376030、化合物

HRID 1871057ノート

反応式

HRID 1871057 の反応式
C(Cl)Cl.C[O:5][C:6]1[C:7]([CH3:17])=[C:8]([CH:13]=[CH:14][C:15]=1[CH3:16])[C:9]([O:11][CH3:12])=[S:10].B(Br)(Br)Br>CO>[OH:5][C:6]1[C:7]([CH3:17])=[C:8]([CH:13]=[CH:14][C:15]=1[CH3:16])[C:9]([O:11][CH3:12])=[S:10]

参加物

5

反応物 3

HCID 6344Dichloromethane2 回HCID 25134Boron tribromideHCID 54217787HCID 54217787、化合物

生成物 1

HCID 54376030HCID 54376030、化合物収率 98%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 90 ml methylene chloride, was dissolved methyl 3-methoxy-2-methyl-4-methylthiobenzoate in an amount of 10 g (0.044 mole), and the resulting solution was then fed dropwise into 90 ml methylene chloride solution of boron tribromide in an amount of 8.4 ml (0.088 mole) at a temperature ranging from 5 to 10° C. After stirring the mixture for 4 hours at an ambient temperature, the mixture was further fed dropwise with 50 ml methanol under cooling with ice and washed with water and then with saturated saline solution. After drying the mixture with anhydrous magnesium sulfate, the solvent remained therein was distillated out under reduced pressure to obtain methyl 3-hydroxy-2-methyl-4-methylthiobenzoate in an amount of 9.2 g. The yield was 98%.

後処理

  1. customranging from 5 to 10° C
  2. temperatureunder cooling with ice
  3. washwashed with water
  4. dry with materialAfter drying the mixture with anhydrous magnesium sulfate

出典と根拠

ORDレコード
ord-82bb3b75e7b842a0b29f94097e9b28be
出典データセット
uspto-grants-2000_08
特許番号
US06100421

反応ノート

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