Dichloromethane → HCID 68532958, 화합물

HRID 657546노트

반응식

HRID 657546 반응식
[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

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 83372Dimethylsulphamoyl chlorideHCID 12159643HCID 12159643, 화합물

생성물 1

HCID 68532958HCID 68532958, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d1d0117bf2874eaf9d2558621b4a15b1
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076325B2

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