Dichloromethane → HCID 68532958、化合物

HRID 657546ノート

反応式

HRID 657546 の反応式
[OH:1][C:2]1[CH:3]=[C:4]2[C:7](=[CH:8][CH:9]=1)[CH:6]([C:10]#[N:11])[CH2:5]2.ClCCl.C(N(CC)CC)C.[CH3:22][N:23]([CH3:28])[S:24](Cl)(=[O:26])=[O:25]>O>[CH3:22][N:23]([CH3:28])[S:24](=[O:26])(=[O:25])[O:1][C:2]1[CH:3]=[C:4]2[C:7](=[CH:8][CH:9]=1)[CH:6]([C:10]#[N:11])[CH2:5]2

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 83372Dimethylsulphamoyl chlorideHCID 12159643HCID 12159643、化合物

生成物 1

HCID 68532958HCID 68532958、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2 g (13.8 mmoles) of 3-hydroxy-bicyclo[4.2.0]octa-1,3,5-triene-7-carbonitrile are mixed into 40 mL of dichloromethane, 3.9 g (2 equivalents) of triethylamine and 1.63 mL (1. 1 equivalents) of dimethylsulphamoyl chloride. Stirring is carried out at 25° C. for 4 days. The reaction mixture is poured into water, extracted with dichloromethane, dried over MgSO4, filtered and evaporated to obtain an oil. This residue is purified by flash chromatography over 70 g of silica (eluant: dichloromethane/toluene: 50/50). The expected product is obtained in the form of a white solid.

後処理

  1. extractionextracted with dichloromethane
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. customevaporated
  5. customto obtain an oil
  6. customThis residue is purified by flash chromatography over 70 g of silica (eluant: dichloromethane/toluene: 50/50)

出典と根拠

ORDレコード
ord-d1d0117bf2874eaf9d2558621b4a15b1
出典データセット
uspto-grants-2011_12
特許番号
US08076325B2

反応ノート

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