O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborate → HCID 68855620, 화합물

HRID 1071679노트

반응식

HRID 1071679 반응식
[Cl:1][C:2]1[S:6][C:5]([C:7]2[O:11][N:10]=[C:9]([CH2:12][N:13]3[C:21]4[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=4)[CH:15]=[C:14]3[C:22](O)=[O:23])[CH:8]=2)=[CH:4][CH:3]=1.[B-](F)(F)(F)F.CCOC(C(C#N)=NOC(N(C)C)=[N+](C)C)=O.[C:47]([O:51][C:52]([N:54]1[CH2:59][CH2:58][N:57]([NH2:60])[CH2:56][CH2:55]1)=[O:53])([CH3:50])([CH3:49])[CH3:48]>C(Cl)Cl>[C:47]([O:51][C:52]([N:54]1[CH2:59][CH2:58][N:57]([NH:60][C:22]([C:14]2[N:13]([CH2:12][C:9]3[CH:8]=[C:7]([C:5]4[S:6][C:2]([Cl:1])=[CH:3][CH:4]=4)[O:11][N:10]=3)[C:21]3[C:16]([CH:15]=2)=[CH:17][CH:18]=[CH:19][CH:20]=3)=[O:23])[CH2:56][CH2:55]1)=[O:53])([CH3:50])([CH3:48])[CH3:49]

참가 물질

5

반응물 3

HCID 2733286O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 11222093HCID 11222093, 화합물HCID 22029174tert-Butyl 4-aminopiperazine-1-carboxylate

생성물 1

HCID 68855620HCID 68855620, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1 g 1-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-1H-indole-2-carboxylic acid and 1.3 ml NEM in 8 ml DCM, 914 mg TOTU were added and the mixture was stirred for 30 min at RT. Then 673 mg 4-Amino-piperazine-1-carboxylic acid tert-butyl ester were added and the reaction was stirred over night. After removal of the solvent under reduced pressure the residue was directly purified by chromatography on silica gel eluting with an ethyl acetate/heptane gradient. Yield: 1.1 g.

후처리

  1. stirringthe reaction was stirred over night
  2. customAfter removal of the solvent under reduced pressure the residue
  3. customwas directly purified by chromatography on silica gel eluting with an ethyl acetate/heptane gradient

출처 및 근거

ORD 기록
ord-bcbddee132e343a4bb5cce235c9b0767
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06906084B2

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