Triethylamine → HCID 68575706, 화합물

HRID 1797264

반응식

HRID 1797264 반응식
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:14][CH3:15])=[C:7](/[CH:9]=[CH:10]/[C:11]([OH:13])=O)[CH:8]=1)#[N:2].C(N(CC)CC)C.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.[CH2:45]([O:52][C:53](=[O:72])[CH2:54][C@@H:55]([NH2:71])[CH2:56][N:57]1[CH2:62][CH2:61][CH:60]([O:63][C:64]2[CH:69]=[CH:68][C:67]([F:70])=[CH:66][CH:65]=2)[CH2:59][CH2:58]1)[C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1>C(Cl)Cl>[CH2:45]([O:52][C:53](=[O:72])[CH2:54][C@@H:55]([NH:71][C:11](=[O:13])/[CH:10]=[CH:9]/[C:7]1[CH:8]=[C:3]([C:1]#[N:2])[CH:4]=[CH:5][C:6]=1[O:14][CH3:15])[CH2:56][N:57]1[CH2:58][CH2:59][CH:60]([O:63][C:64]2[CH:65]=[CH:66][C:67]([F:70])=[CH:68][CH:69]=2)[CH2:61][CH2:62]1)[C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 11458357(E)-3-(5-cyano-2-methoxy-phenyl)-acrylic acidHCID 68576481HCID 68576481, 화합물

생성물 1

HCID 68575706HCID 68575706, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of (E)-3-(5-cyano-2-methoxy-phenyl)-acrylic acid (0.916 g, 4.51 mmol), triethylamine (1.257 ml, 9.02 mmol) and 2-(1H-benzotriazol-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (1.44 g, 4.51 mmol) in DCM (10 ml) is treated with (R)-3-amino-4-[4-(4-fluoro-phenoxy)-piperidin-1-yl]-butyric acid benzyl ester. The reaction mixture is stirred at ambient temperature for 2 hours, then is washed with water, dried over MgSO4 and evaporated. The crude product is purified by flash silica chromatography (elution with 2:1 ethylacetate:hexane) to afford (R)-3-[(E)-3-(5-cyano-2-methoxy-phenyl)-acryloylamino]-4-[4-(4-fluoro-phenoxy)-piperidin-1-yl]-butyric acid benzyl ester. [MH]+ 572.1.

후처리

  1. washis washed with water
  2. dry with materialdried over MgSO4
  3. customevaporated
  4. customThe crude product is purified by flash silica chromatography (elution with 2:1 ethylacetate:hexane)

출처 및 근거

ORD 기록
ord-f2098ee258b54dee8f28f07d97d8407b
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07034042B2

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