Hydrochloric Acid → p-(Octylthiomethyl)benzyl chloride

HRID 8423

反応式

HRID 8423 の反応式
CC(C)([O-])C.[Na+].[CH2:7]([SH:15])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[C:16]1([CH2:24]Cl)[CH:21]=[CH:20][C:19]([CH2:22][Cl:23])=[CH:18][CH:17]=1.Cl>CO>[CH2:7]([S:15][CH2:24][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][Cl:23])=[CH:18][CH:17]=1)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 81441-OctanethiolHCID 12171alpha,alpha'-Dichloro-p-xyleneHCID 23676156Sodium t-butoxide

生成物 1

HCID 10613099p-(Octylthiomethyl)benzyl chloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

1.83 g (19 mmol) of sodium t-butoxide and 2.78 g (19 mmol) of octanethiol were stirred into 40 g of methanol at room temperature. After 30 minutes, the clear solution was added in one portion to 3.33 g (19 mmol) of p-xylylene dichloride in 100 g of methanol. After one hour, the mixture was neutralized using 1N hydrochloric acid, and all the volatile components were removed under reduced pressure. The crude product was taken up in 250 ml of chloroform and washed twice with 100 ml of water each time, dried and evaporated under reduced pressure. 5.29 g, which, according to 1H-NMR-spectroscopy, consisted of 50% of product, 25% of starting material and 25% of p-bis(octylthiomethyl)benzene.

後処理

  1. waitAfter one hour
  2. customall the volatile components were removed under reduced pressure
  3. washwashed twice with 100 ml of water each time
  4. customdried
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-1dafe2e64013446290804c2d6d9417a2
出典データセット
uspto-grants-2006_08
特許番号
US07087787B1

関連ノート

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