Triethylamine → HCID 58834669、化合物

HRID 1443826ノート

反応式

HRID 1443826 の反応式
[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

参加物

6

反応物 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

生成物 1

HCID 58834669HCID 58834669、化合物収率 45%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-afbe9b4308ef48e18e33f05c521ec51a
出典データセット
uspto-grants-2010_02
特許番号
US07662824B2

反応ノート

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