Citric Acid → HCID 54268940, 화합물

HRID 1683051노트

반응식

HRID 1683051 반응식
[CH2:1]([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)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH2:29](Br)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CN(C=O)C>[CH2:29]([N:13]1[C:12](=[O:24])[C:11]2([CH2:25][CH2:26][N:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH2:9][CH2:10]2)[N:15]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[C:14]1=[O:23])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1

참가 물질

6

반응물 4

HCID 311Citric Acid2회HCID 7498Benzyl BromideHCID 24758Sodium hydrideHCID 53759290HCID 53759290, 화합물

생성물 1

HCID 54268940HCID 54268940, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Combine 8-benzyl-1-(4-fluoro-phenyl)-1,3,8-triaza-spiro[4.5]decane-2,4-dione (12 mmol) and DMF (20 mL). Cool in an ice bath. Add NaH (18 mmol) in several portions. After the addition is complete, add benzyl bromide (18 mmol). Allow the reaction mixture to warm to ambient temperature. After 3 h, cool the reaction vessel using an ice bath and cautiously add 10% aqueous citric acid (20 mL). When gas evolution has ceased, pour into an additional 20 mL of 10% aqueous citric acid and extract using ethyl acetate (3×60 mL). Extract the combined organics with saturated aqueous NaCl, dry over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Purify to obtain the title compound.

후처리

  1. temperatureCool in an ice bath
  2. additionAfter the addition
  3. temperaturecool the reaction vessel
  4. extractionextract
  5. extractionExtract the combined organics with saturated aqueous NaCl
  6. dry with materialdry over Na2SO4
  7. filtrationfilter
  8. concentrationconcentrate in vacuo
  9. customto obtain a residue
  10. customPurify

출처 및 근거

ORD 기록
ord-f78632f6abac4b7fa737f8f91fcdb495
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05635510

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