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Tributylborane → 4-[6-(4-Fluorophenyl)spiro[2.4]hept-5-en-5-yl]benzenesulfonamide

HRID 2292984
ノート
印刷プレビュー

反応式

HRID 2292984 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:9][C:10]3([CH2:13][C:14]=2[C:15]2[CH:20]=[CH:19][C:18]([S:21](C)(=[O:23])=[O:22])=[CH:17][CH:16]=2)[CH2:12][CH2:11]3)=[CH:4][CH:3]=1.C[Li].C(B(CCCC)CCCC)CCC.C([O-])(=O)C.[Na+].[NH2:45]OS(O)(=O)=O>C1COCC1.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:9][C:10]3([CH2:12][CH2:11]3)[CH2:13][C:14]=2[C:15]2[CH:20]=[CH:19][C:18]([S:21]([NH2:45])(=[O:23])=[O:22])=[CH:17][CH:16]=2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 31216TributylboraneHCID 76284hydroxylamine-O-sulfonic acidHCID 517045Sodium AcetateHCID 98517705-(4-Fluorophenyl)-6-(4-methylsulfonylphenyl)spiro[2.4]hept-5-eneHCID 178418348HCID 178418348、化合物

生成物 1

HCID 99280474-[6-(4-Fluorophenyl)spiro[2.4]hept-5-en-5-yl]benzenesulfonamide
収率 28.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Under nitrogen, a solution of 90 mg (0.248 mmol) of 5-(4-fluoro phenyl)-6-[4-(methylsulfonyl)phenyl]spiro[2.4]hept-5-ene from step 11 in 1 mL of THF at -78° C. was treated with 0.21 mL (0.27 mmol) of methyllithium (1.3M in ether) over a period of 2 minutes. The reaction was stirred at ambient temperature for 25 minutes, cooled to -78° C., and treated with 0.3 mL (0.3 mmol) of tributylborane (1.0M in THF). The resulting dark brown solution was stirred at ambient temperature for 20 minutes and then at reflux for 16 hour prior to the addition of 350 mg (4.27 mmol) of sodium acetate, 2 mL of water, and 250 mg (2.21 mmol) of hydroxylamine-O-sulfonic acid. The resulting light orange mixture was stirred at ambient temperature for 3 hours and the aqueous phase extracted with ethyl acetate. The combined extracts were washed with water, brine, dried (MgSO4), and concentrated in vacuo. The residue was chromatographed on silica gel to give 24 mg (27%) of 4-[6-(4-fluorophenyl)spiro[2.4]hept-5-en-5-yl]benzenesulfonamide as a colorless solid: mp 131.0°-133.0° C.; NMR (CDCl3) δ 0.68 (s, 4H), 2.90 (s, 3H), 4.81 (s, 2H), 6.92 (t, J=9 Hz, 2H), 7.11 (dd, J=6 and 9 Hz, 2H), 7.27 (d, J=9 Hz, 2H), 7.74 (d, J=9 Hz, 2H). HRMS. Calc'd for C19H18FNO2S: 344.1121. Found: 344.1122. Anal. Calc'd for [C19H18FNO2S+0.1 CH3CO2 CH2CH3 ]: C, 66.16; H, 3.98; S, 9.11. Found: C, 65.86; H, 5.52; N, 3.92; S, 9.57.

後処理

  1. temperaturecooled to -78° C.
  2. stirringThe resulting dark brown solution was stirred at ambient temperature for 20 minutes
  3. temperatureat reflux for 16 hour
  4. stirringThe resulting light orange mixture was stirred at ambient temperature for 3 hours
  5. extractionthe aqueous phase extracted with ethyl acetate
  6. washThe combined extracts were washed with water, brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo
  9. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-4fb3e72e48474794ae5c6181159a5966
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05684195

反応ノート

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