1,2-Dichloroethane → HCID 54297219, 화합물

HRID 1683053노트

반응식

HRID 1683053 반응식
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

참가 물질

5

반응물 3

HCID 111,2-DichloroethaneHCID 5213051-Chloroethyl chloroformateHCID 53759290HCID 53759290, 화합물

생성물 1

HCID 54297219HCID 54297219, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5cb933a4d7fd476ea85a5958d8dbbc79
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05635510

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