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Diisopropylethylamine → HCID 86719164, 화합물

HRID 2172695
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HRID 2172695 반응식
[F:1][C:2]([F:18])([F:17])[C:3]1[O:7][N:6]=[C:5]([C:8]2[CH:16]=[CH:15][C:11]([C:12]([OH:14])=O)=[CH:10][CH:9]=2)[N:4]=1.CCOC(C(C#N)=NOC(N1CCOCC1)=[N+](C)C)=O.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[C:55]([N:62]([CH3:66])[CH2:63][CH2:64][NH2:65])([O:57][C:58]([CH3:61])([CH3:60])[CH3:59])=[O:56]>C(Cl)Cl>[CH3:66][N:62]([CH2:63][CH2:64][NH:65][C:12](=[O:14])[C:11]1[CH:10]=[CH:9][C:8]([C:5]2[N:4]=[C:3]([C:2]([F:1])([F:18])[F:17])[O:7][N:6]=2)=[CH:16][CH:15]=1)[C:55](=[O:56])[O:57][C:58]([CH3:61])([CH3:59])[CH3:60]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 2756424N-Boc-N-methylethylenediamineHCID 104914054-(5-(Trifluoromethyl)-1,2,4-oxadiazol-3-yl)benzoic acidHCID 75951468(1-Cyano-2-ethoxy-2-oxoethylidenaminooxy)dimethylamino-morpholino-carbenium hexafluorophosphate

생성물 1

HCID 86719164HCID 86719164, 화합물

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To a suspension of 4-(5-(trifluoromethyl)-1,2,4-oxadiazol-3-yl)benzoic acid (1 g, 3.87 mmol) in DCM (10 ml) was added COMU (1.825 g, 4.26 mmol) and DIPEA (0.812 ml, 4.65 mmol). The yellow solution was stirred for 2 min at rt and turned red. N-Boc-N-methyl-ethylenediamine (0.810 g, 4.65 mmol) was added and the reaction mixture was stirred at reflux for 1 hr, allowed to cool to rt and washed with water, saturated aqueous NH4Cl, and extracted with EtOAc. The organic layer was dried over Na2SO4 and the solvent was removed in vacuum. The final product was purified according to Method B in Examples 124-156 general method.

후처리

  1. stirringthe reaction mixture was stirred
  2. temperatureat reflux for 1 hr
  3. temperatureto cool to rt
  4. washwashed with water, saturated aqueous NH4Cl
  5. extractionextracted with EtOAc
  6. dry with materialThe organic layer was dried over Na2SO4
  7. customthe solvent was removed in vacuum
  8. customThe final product was purified

출처 및 근거

ORD 기록
ord-38e2b722836b46d7a4cabfc2d09a877e
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056843B2

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