Triethylamine → HCID 58834669, 화합물

HRID 1443826노트

반응식

HRID 1443826 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[Br:8][C:9]1[CH:17]=[C:16]([C:18]([OH:20])=O)[CH:15]=[C:14]2[C:10]=1[CH:11]=[CH:12][NH:13]2.C(N(CC)CC)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C>[Br:8][C:9]1[CH:17]=[C:16]([C:18]([N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]2)=[O:20])[CH:15]=[C:14]2[C:10]=1[CH:11]=[CH:12][NH:13]2

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 531671-MethylpiperazineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 247286084-Bromo-1H-indole-6-carboxylic acid

생성물 1

HCID 58834669HCID 58834669, 화합물수율 45%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-Methyl-piperazine (0.21 g, 2.1 mmol) was added to a solution of 4-bromo-1H-indole-6-carboxylic acid (0.50 g, 2.1 mmol), triethylamine (0.43 mL, 3.1 mmol) and HBTU (0.78 g, 2.1 mmol) in DMF (5 mL) and stirred at room temperature overnight. Reaction mixture was concentrated in vacuo and purified by column chromatography (10% methanol in dichloromethane) to yield 0.30 g (45%) of (4-bromo-1H-indol-6-yl)-(4-methyl-piperazin-1-yl)-methanone. Mass spectrum (LCMS, ESI pos.): Calcd for C14H16BrN3O: 321.05. Found 322.0 ; (M+H).

후처리

  1. customReaction mixture
  2. concentrationwas concentrated in vacuo
  3. custompurified by column chromatography (10% methanol in dichloromethane)

출처 및 근거

ORD 기록
ord-afbe9b4308ef48e18e33f05c521ec51a
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07662824B2

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