Tetrahydrothiophene → HCID 86604150, 화합물

HRID 2068467노트

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HRID 2068467 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 86604150HCID 86604150, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-33781b762ada4e5986bd69a3200b7b09
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08298830B2

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