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1-Methylpiperazine → 3-Methoxy-4-[(trimethylsilyl)ethynyl]phenyl-4-methylpiperazine

HRID 1403208
ノート
印刷プレビュー

反応式

HRID 1403208 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][Si:10]([CH3:13])([CH3:12])[CH3:11])=[C:4]([O:14][CH3:15])[CH:3]=1.[Li+].C[Si]([N-][Si](C)(C)C)(C)C.[CH3:26][N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1>C1COCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(P(C2CCCCC2)C2(N(C)C)CC=CC=C2C2C=CC=CC=2)CCCCC1>[CH3:15][O:14][C:4]1[CH:3]=[C:2]([N:30]2[CH2:31][CH2:32][N:27]([CH3:26])[CH2:28][CH2:29]2)[CH:7]=[CH:6][C:5]=1[C:8]#[C:9][Si:10]([CH3:13])([CH3:12])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 531671-MethylpiperazineHCID 2733832Lithium HexamethyldisilazideHCID 71239496[(4-Bromo-2-methoxyphenyl)ethynyl](trimethyl)silane

生成物 1

HCID 867252923-Methoxy-4-[(trimethylsilyl)ethynyl]phenyl-4-methylpiperazine収率 68.4%

試薬・触媒・溶媒 3

HCID 9811564Bis(dibenzylideneacetone)palladium
触媒
HCID 665453382-Dicyclohexylphosphino-2-(N,N-Dimethylamino)Biphenyl触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of [(4-bromo-2-methoxyphenyl)ethynyl](trimethyl)silane (1.426 g, 5.035 mmol) in dry THF (25 mL) was degassed and backfilled with argon for three times. Pd2(dba)3 (230.5 mg, 0.252 mmol) and 2-dicyclohexylphosphino-2-(N,N′-dimethylamino)biphenyl (79.3 mg, 0.201 mmol) were added under argon atmosphere and the mixture was degassed and backfilled with argon for three times. Then 1 M LiHMDS in THF (12.1 mL, 12.084 mmol) and N-methylpiperazine (1.34 mL, 1.21 g, 12.083 mmol) were added by a syringe and the mixture was degassed and backfilled with Argon for three times. The reaction mixture was heated to reflux for 1 h. After cooling to room temperature the reaction mixture was filtered on a pad of celite washing with THF (200 mL). The filtrate was evaporated under vacuum and the black oil so obtained was purified by chromatography on silica gel (DCM/MeOH 9/1) to afford the title compound as a brownish solid (1.042 g, 68.4%).

後処理

  1. customthe mixture was degassed
  2. customthe mixture was degassed
  3. temperatureThe reaction mixture was heated
  4. temperatureto reflux for 1 h
  5. filtrationwas filtered on a pad of celite
  6. washwashing with THF (200 mL)
  7. customThe filtrate was evaporated under vacuum
  8. customthe black oil so obtained
  9. customwas purified by chromatography on silica gel (DCM/MeOH 9/1)

出典と根拠

ORDレコード
ord-2647c7aa74384512ad91b54f599d80a0
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08912200B2

反応ノート

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