Methyl 3-methyl-6-(phenylthio)-benzoate → HCID 12539099、化合物

HRID 435664ノート

反応式

HRID 435664 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:9]([S:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:10][CH:11]=1)[C:5](OC)=[O:6]>O1CCCC1.C1C=CC=CC=1.Cl>[CH3:1][C:2]1[CH:3]=[C:4]([C:9]([S:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:10][CH:11]=1)[CH2:5][OH:6]

参加物

5

反応物 1

HCID 21481132Methyl 3-methyl-6-(phenylthio)-benzoate

生成物 1

HCID 12539099HCID 12539099、化合物

試薬・触媒・溶媒 3

HCID 241Benzene溶媒2 回HCID 313Hydrochloric Acid溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

322.5 g of methyl 3-methyl-6-(phenylthio)-benzoate in 3 litres of absolute tetrahydrofuran are treated dropwise over a period of 30 minutes under argon and under reflux with 420 ml of a 70% sodium-dihydro-bis(2-methoxyethoxy)-aluminate solution in benzene and the mixture is boiled for a further 3 hours under reflux. Then the mixture is cooled to ca 4° C, diluted with 1 litre of benzene, hydrolysed with 700 ml of 2-N hydrochloric acid, then poured on to ice-water and treated with a further 400 ml of concentrated hydrochloric acid in order to obtain a clear solution. The organic phase is washed with water, dried over sodium sulphate, filtered and evaporated. There is obtained 3-methyl-6-(phenylthio)-benzyl alcohol as a red-brown oil.

後処理

  1. temperatureunder reflux
  2. temperatureThen the mixture is cooled to ca 4° C
  3. customto obtain a clear solution
  4. washThe organic phase is washed with water
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-090467a5b32441e2a20ef71aee92d5fe
出典データセット
uspto-grants-1977_02
特許番号
US04006144

反応ノート

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