Dimethyl Sulfoxide → HCID 9819244、化合物

HRID 1274308ノート

反応式

HRID 1274308 の反応式
C(Cl)(=O)C(Cl)=O.CS(C)=O.[CH3:11][C:12]1[C:13]([S:26][C:27]2[CH:32]=[CH:31][C:30]([CH2:33][OH:34])=[CH:29][CH:28]=2)=[CH:14][C:15]2[C:16]([CH3:25])([CH3:24])[CH2:17][CH2:18][C:19]([CH3:23])([CH3:22])[C:20]=2[CH:21]=1.C(N(CC)CC)C>ClCCl.O>[CH3:11][C:12]1[C:13]([S:26][C:27]2[CH:32]=[CH:31][C:30]([CH:33]=[O:34])=[CH:29][CH:28]=2)=[CH:14][C:15]2[C:16]([CH3:25])([CH3:24])[CH2:17][CH2:18][C:19]([CH3:22])([CH3:23])[C:20]=2[CH:21]=1

参加物

7

反応物 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 9840907HCID 9840907、化合物

生成物 1

HCID 9819244HCID 9819244、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

60 μl (0.7 mmol) of oxalyl chloride and 5 ml of dichloromethane were introduced into a three-necked flask and under a nitrogen stream. 100 Al (1.4 mmol) of DMSO were added at -60° C. and the mixture was stirred for 10 min and then a solution of 200 mg (0.6 mmol) of 4-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-2-naphthylthio)benzenemethanol in 5 ml of dichloromethane and 400 μl (3 mmol) of triethylamine was added. The mixture was stirred at room temperature for one hour, the reaction medium poured into water, extracted with dichloromethane, the organic phase decanted off, dried over magnesium sulfate and evaporated.

後処理

  1. stirringThe mixture was stirred at room temperature for one hour
  2. customthe reaction
  3. extractionextracted with dichloromethane
  4. customthe organic phase decanted off
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

出典と根拠

ORDレコード
ord-e46399fe899a45e0a22294346ec111db
出典データセット
uspto-grants-2000_12
特許番号
US06156788

反応ノート

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