Tributyl(2-phenylethynyl)stannane → HCID 86601214, 화합물

HRID 349257

반응식

HRID 349257 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 86601214HCID 86601214, 화합물수율 88%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-69c4d2941ae84e44bf928c2351a234b2
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179804B2

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