Dichloromethane → HCID 71245552, 화합물

HRID 575497노트

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HRID 575497 반응식
C(O[CH:4](OCC)[CH2:5][S:6][C:7]1[C:16]([O:17][CH3:18])=[CH:15][C:14]2[C:9](=[CH:10][C:11]([O:28][CH3:29])=[C:12]([S:19][CH2:20][CH:21](OCC)OCC)[CH:13]=2)[CH:8]=1)C.ClC1C=CC=CC=1.ClCCl>CO>[CH3:29][O:28][C:11]1[C:12]2[S:19][CH:20]=[CH:21][C:13]=2[C:14]2[CH:15]=[C:16]([O:17][CH3:18])[C:7]3[S:6][CH:5]=[CH:4][C:8]=3[C:9]=2[CH:10]=1

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 7964ChlorobenzeneHCID 866765302,6-Bis-(2,2-diethoxy-ethylsulfanyl)-3,7-dimethoxy-naphthalene

생성물 1

HCID 71245552HCID 71245552, 화합물수율 66%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
140 °C

실험 절차

Compound 6 (5.0 g, 10.3 mmol) and 6.8 g of 84% polyphorphoric acid were added into a 250 mL 3-neck flask equipped with a condenser. The system was flashed with argon for 15 minutes before 50 mL of anhydrous chlorobenzene was added. The mixture was heated at 140° C. for 40 hours before it was cooled down to room temperature. Dichloromethane (100 mL) was added. The organic mixture was washed with saturated NaHCO3 before the solvent was removed under vacuum. Methanol (100 mL) was added before compound 7 (2.0 g, ˜66% yield) was collected as a white solid by filtration, washed with methanol and dried in vacuo. 1H NMR (CDCl3, 500 MHz): δ 7.97 (d, 2H, J=5.5 Hz), δ 7.62 (d, 2H, J=5.5 Hz), 67.51 (s, 2H), δ 4.18 (s, 6H).

후처리

  1. customequipped with a condenser
  2. additionwas added
  3. temperaturewas cooled down to room temperature
  4. washThe organic mixture was washed with saturated NaHCO3 before the solvent
  5. customwas removed under vacuum

출처 및 근거

ORD 기록
ord-3af71bcf06de461e9661449fafd65b21
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09035004B2

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