Tetrahydrothiophene → HCID 86604150、化合物

HRID 2068467ノート

反応式

HRID 2068467 の反応式
[S:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1.[F:6][C:7]([F:23])([F:22])[C:8]1[CH:13]=[C:12]([CH2:14][Br:15])[C:11]([C:16]([F:19])([F:18])[F:17])=[CH:10][C:9]=1[CH2:20]Br>CO>[Br-:15].[Br-:15].[F:6][C:7]([F:23])([F:22])[C:8]1[CH:13]=[C:12]([CH2:14][S+:1]2[CH2:5][CH2:4][CH2:3][CH2:2]2)[C:11]([C:16]([F:19])([F:18])[F:17])=[CH:10][C:9]=1[CH2:20][S+:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 1127TetrahydrothiopheneHCID 592605761,4-Bis(bromomethyl)-2,5-bis(trifluoromethyl)benzene

生成物 1

HCID 86604150HCID 86604150、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

Tetrahydrothiophene (0.27 mL, 3 mmol) was added to a suspension of compound 24 (200 mg, 0.5 mmol) in dry methanol (5 mL). The solid was dissolved to form a clear solution within 10 min. This solution was filtered via 0.45 μm membrane filter and then heated to 50° C. with stirring for 24 h. After cooling down to room temperature, the solvent was completely removed in vacuo and cold acetone (10 mL) was added to the residue. The precipitate was then filtered and dried to give compound 217a as a colorless, hygroscopic solid (192 mg, 67%): 1H NMR (300 MHz, D2O): 8.17 (2H, s), 4.76 (4H, s), 3.52-3.62 (8H, m), 2.34-2.47 (8H, m); 19F NMR (282 MHz, D2O): −60.2; HR-MS (EI) calcd. for C18H22F6S2Br2 (M+): 573.94, found ([M−Br]+): 495.04.

後処理

  1. dissolutionThe solid was dissolved
  2. customto form a clear solution within 10 min
  3. filtrationThis solution was filtered via 0.45 μm membrane
  4. filtrationfilter
  5. temperatureAfter cooling down to room temperature
  6. customthe solvent was completely removed in vacuo and cold acetone (10 mL)
  7. additionwas added to the residue
  8. filtrationThe precipitate was then filtered
  9. customdried

出典と根拠

ORDレコード
ord-33781b762ada4e5986bd69a3200b7b09
出典データセット
uspto-grants-2012_10
特許番号
US08298830B2

反応ノート

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