Tributyl(2-phenylethynyl)stannane → HCID 86601214、化合物

HRID 349257

反応式

HRID 349257 の反応式
[CH2:1]([Sn:5]([CH2:18][CH2:19][CH2:20][CH3:21])([CH2:14][CH2:15][CH2:16][CH3:17])[C:6]#[C:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH2:2][CH2:3][CH3:4].[F:22][C:23]([F:39])([F:38])[C:24]1[CH:25]=[C:26]([CH:31]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:33]=1)[CH2:27][N:28]=[N+:29]=[N-:30]>C1(C)C=CC=CC=1>[F:22][C:23]([F:38])([F:39])[C:24]1[CH:25]=[C:26]([CH:31]=[C:32]([C:34]([F:37])([F:35])[F:36])[CH:33]=1)[CH2:27][N:28]1[C:7]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)=[C:6]([Sn:5]([CH2:1][CH2:2][CH2:3][CH3:4])([CH2:14][CH2:15][CH2:16][CH3:17])[CH2:18][CH2:19][CH2:20][CH3:21])[N:30]=[N:29]1

参加物

4

反応物 2

HCID 630640Tributyl(2-phenylethynyl)stannaneHCID 441857431-(Azidomethyl)-3,5-bis(trifluoromethyl)benzene

生成物 1

HCID 86601214HCID 86601214、化合物収率 88%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Heat a mixture of tri-n-butyl-phenylethynyl-stannane (11.0 g, 30.0 mmol) and 3,5-bis-trifluoromethyl-benzyl azide (9.68 g, 36.0 mmol) in toluene (40 mL) at reflux until reaction is complete. Concentrate to remove the solvent in vacuo and purify the residue by flash chromatography on silica gel (elution with 17% ether in hexanes) to give the title compound (17.5 g, 26.4 mmol, 88%). MS (ES) 660.1, 662.1 (M+1); LC Rf=0.1 (17% ether in hexanes).

後処理

  1. temperatureHeat
  2. temperatureat reflux until reaction
  3. concentrationConcentrate
  4. customto remove the solvent in vacuo
  5. custompurify the residue by flash chromatography on silica gel (elution with 17% ether in hexanes)

出典と根拠

ORDレコード
ord-69c4d2941ae84e44bf928c2351a234b2
出典データセット
uspto-grants-2007_02
特許番号
US07179804B2

関連ノート

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