Methanol → HCID 178527782, 화합물

HRID 359920

반응식

HRID 359920 반응식
CO[C:3]1[C:4](=O)[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.[NH2:11][C:12]([NH2:14])=[S:13].C[O-].[Na+].CO.CO>C(O)(=O)C>[SH:13][C:12]1[N:11]=[C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=[C:3]2[N:14]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 165462-Methoxy-2,4,6-cycloheptatrien-1-oneHCID 2723790ThioureaHCID 23694274Sodium methanolate methanol

생성물 1

HCID 178527782HCID 178527782, 화합물수율 70%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

In accordance with the method described in Journal of the Americal Chemical Society, Vol. 76, pages 3352 to 3353 (1954), 150 g of 2-methoxy-2,4,6-cycloheptatrien-1-one and 84 g of thiourea were added to 255 g of 28% sodium methoxide/methanol solution and stirred for 30 minutes at room temperature. Further, 600 ml of methanol was added and acetic acid was added until the pH of the resulting solution became 5 or so. The crystals precipitated were separated by filtration and washed with methanol. Next, the thus obtained crystals were added to one liter of methanol and heated under reflux for 30 minutes. After cooling to room temperature, the crystals were separated by filtration and then dried. 125 g of yellow crystals was obtained.

후처리

  1. customThe crystals precipitated
  2. customwere separated by filtration
  3. washwashed with methanol
  4. additionNext, the thus obtained crystals were added to one liter of methanol
  5. temperatureheated
  6. temperatureunder reflux for 30 minutes
  7. temperatureAfter cooling to room temperature
  8. customthe crystals were separated by filtration
  9. customdried

출처 및 근거

ORD 기록
ord-eb03c6b574f5401bb319c4b39ea4d071
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05003077

연결된 노트

불러오는 중…