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Triethylamine → HCID 20439515, 화합물

HRID 1979599
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HRID 1979599 반응식
[CH3:1][CH:2]1[CH2:6][N:5]([C:7]2[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=2)[NH:4][C:3]1=[O:14].[Si:15](Cl)([C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:17])[CH3:16].C(N(CC)CC)C.N12CCCN=C1CCCCC2>C1(C)C=CC=CC=1.CN(C1C=CN=CC=1)C>[CH3:1][CH:2]1[CH2:6][N:5]([C:7]2[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=2)[N:4]=[C:3]1[O:14][Si:15]([C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:17])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 28928tert-Butyldimethylsilyl chlorideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 222232384-Methyl-1-(4-methylphenyl)-3-pyrazolidinone

생성물 1

HCID 20439515HCID 20439515, 화합물수율 98%

시약·촉매·용매 2

HCID 14284
4-(Dimethylamino)pyridine
촉매
HCID 1140Toluene용매

실험 절차

To a stirred solution under nitrogen of 4-methyl-1-p-tolyl-3-pyrazolidinone (19.0 g, 0.10 mole) and t-butyldimethylsilyl chloride (16.6 g, 0.11 mole) in 200 ml toluene, was added sequentially triethylamine (10.6 g, 0.11 mole), 1,8-diazabicyclo- [5.4.0]-undec-7-ene (0.1 g), and 4-(N,N-dimethylamino) pyridine (0.1 g). The mixture was refluxed for 16 hours, cooled to room temperature and filtered. The salts were washed with ether and the solvents of the combined filtrate were removed under reduced pressure. The resulting residue was treated with 200 ml adhydrous ether, filtered to remove salts, and dried over anhydrous magnesium sulfate. Removal of the solvent yielded 29.8 g (98% yield).

후처리

  1. temperatureThe mixture was refluxed for 16 hours
  2. filtrationfiltered
  3. washThe salts were washed with ether
  4. customthe solvents of the combined filtrate were removed under reduced pressure
  5. additionThe resulting residue was treated with 200 ml adhydrous ether
  6. filtrationfiltered
  7. customto remove salts
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customRemoval of the solvent
  10. customyielded 29.8 g (98% yield)

출처 및 근거

ORD 기록
ord-5a2ff95311d743dcb583243e6cc5af76
출처 데이터셋
uspto-grants-1984_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04481287

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