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Water → HCID 135966585, 화합물

HRID 1709973
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HRID 1709973 반응식
B(Br)(Br)Br.C[O:6][C:7]1[C:23]([O:24]C)=[CH:22][C:10]2[S:11][C:12]([C:14]3[CH:15]([CH3:21])[CH2:16][C:17](=[O:20])[NH:18][N:19]=3)=[CH:13][C:9]=2[CH:8]=1.O>ClCCl>[OH:6][C:7]1[C:23]([OH:24])=[CH:22][C:10]2[S:11][C:12]([C:14]3[CH:15]([CH3:21])[CH2:16][C:17](=[O:20])[NH:18][N:19]=3)=[CH:13][C:9]=2[CH:8]=1
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참가 물질

5

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HCID 962WaterHCID 25134Boron tribromideHCID 1311006-(5,6-Dimethoxybenzo(b)thien-2-yl)-4,5-dihydro-5-methyl-3(2H)-pyridazinone

생성물 1

HCID 135966585HCID 135966585, 화합물수율 93.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Boron tribromide (1.55 ml) was added to a stirred solution of 4,5-dihydro-6-(5,6-dimethoxy-benzo[b]thien-2-yl)-5-methyl-3(2H)-pyridazinone (1.14 g) in dichloromethane (200 ml). After 2 hours the orange solution was cooled in ice, and water (40 ml) was added. The dichloromethane was then evaporated off under reduced pressure and the residual suspension was filtered to give 4,5-dihydro-6-(5,6-dihydroxy-benzo[b]thien-2-yl)-5-methyl-3(2H)-pyridazinone (0.97 g) as a yellow solid. Crystallisation from dichloromethane:methanol and diethylether gave 4,5-dihydro-6-(5,6-dihydroxybenzo[b]thien-2-yl)-5-methyl-3(2H)-pyridazinone. m.p. >270° C.

후처리

  1. temperatureAfter 2 hours the orange solution was cooled in ice
  2. customThe dichloromethane was then evaporated off under reduced pressure
  3. filtrationthe residual suspension was filtered

출처 및 근거

ORD 기록
ord-c6d0e31000164bceaabc0c91fff603de
출처 데이터셋
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04952571

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