1,2-Dichloroethane → HCID 54297219、化合物

HRID 1683053ノート

反応式

HRID 1683053 の反応式
C([N:8]1[CH2:26][CH2:25][C:11]2([N:15]([C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)[C:14](=[O:23])[NH:13][C:12]2=[O:24])[CH2:10][CH2:9]1)C1C=CC=CC=1.ClCCCl.ClC(OC(Cl)C)=O>CO>[F:22][C:19]1[CH:20]=[CH:21][C:16]([N:15]2[C:11]3([CH2:10][CH2:9][NH:8][CH2:26][CH2:25]3)[C:12](=[O:24])[NH:13][C:14]2=[O:23])=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 111,2-DichloroethaneHCID 5213051-Chloroethyl chloroformateHCID 53759290HCID 53759290、化合物

生成物 1

HCID 54297219HCID 54297219、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Combine 8-benzyl-1-(4-fluoro-phenyl)-1,3,8-triaza-spiro[4.5]decane-2,4-dione (10 mmol) and 1,2-dichloroethane (70 mL). Cool using an ice bath. Add in dropwise fashion, 1-chloroethyl chloroformate (48.6 mmol). Warm to ambient temperature and maintain for 1 h. Extract using saturated NaHCO3 (120 mL). Extract the aqueous phase using dichloromethane (120 mL). Combine the organic layers, extract with saturated NaCl, dry over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Add anhydrous methanol (70 mL) and heat at reflux for 1 h. Concentrate in vacuo to obtain a residue and purify to obtain the title compound.

後処理

  1. temperatureCool
  2. temperaturemaintain for 1 h
  3. extractionExtract
  4. extractionExtract the aqueous phase
  5. extractionCombine the organic layers, extract with saturated NaCl
  6. dry with materialdry over Na2SO4
  7. filtrationfilter
  8. concentrationconcentrate in vacuo
  9. customto obtain a residue
  10. temperatureat reflux for 1 h
  11. concentrationConcentrate in vacuo
  12. customto obtain a residue
  13. custompurify

出典と根拠

ORDレコード
ord-5cb933a4d7fd476ea85a5958d8dbbc79
出典データセット
uspto-grants-1997_06
特許番号
US05635510

反応ノート

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