Hydrochloric Acid → HCID 178447890、化合物

HRID 613189ノート

反応式

HRID 613189 の反応式
[Mg].[CH2:2]([C@H:5]1[CH2:10][CH2:9][C@H:8]([C:11]2[CH:16]=[CH:15][C:14](Br)=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)[CH2:3][CH3:4].[C:18](=[S:20])=[S:19].Cl>C1COCC1>[CH2:2]([C@H:5]1[CH2:10][CH2:9][C@H:8]([C:11]2[CH:16]=[CH:15][C:14]([C:18]([SH:20])=[S:19])=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)[CH2:3][CH3:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6348Carbon DisulfideHCID 5462224MagnesiumHCID 178447827HCID 178447827、化合物

生成物 1

HCID 178447890HCID 178447890、化合物収率 17.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution obtained by suspending 2.25 g (93 mmol) of magnesium in 50 mL of THF, a solution of 20.0 g (71 mmol) of 4-(trans-4-propylcyclohexyl)phenyl bromide in 100 mL of THF was added dropwise with stirring at the room temperature for 45 minutes and stirred with reflux for 30 minutes, to prepare a Grignard reagent. To the solution, 16.3 g (214 mmol) of carbon disulfide was added dropwise for 15 minutes at the room temperature and stirred for one night. To the reaction solution, 60 mL of 3 M hydrochloric acid was added to stop the reaction, extracted with ether, and dried with anhydrous magnesium sulfate. After filtering off magnesium sulfate, the filtrate was concentrated under reduced pressure, to obtain 3.50 g (yield 17.7%) of 4-(trans-4-propylcyclohexyl)phenyl dithiocarboxylic acid.

後処理

  1. customTo a solution obtained
  2. stirringstirred
  3. temperaturewith reflux for 30 minutes
  4. stirringstirred for one night
  5. customthe reaction
  6. extractionextracted with ether
  7. dry with materialdried with anhydrous magnesium sulfate
  8. filtrationAfter filtering off magnesium sulfate
  9. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-4b5b8588eb4a4ea09c62c53a26e20412
出典データセット
uspto-grants-1999_12
特許番号
US06007740

反応ノート

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