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Phenyl isocyanate → HCID 178493809, 화합물

HRID 1528075
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HRID 1528075 반응식
[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6]([O:10][CH3:11])[C:7]=1[O:8]C.N1CCOCC1.C1(N=C=O)C=CC=CC=1>C(OCC)(=O)C>[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6]([O:10][CH3:11])[C:7]=1[OH:8]
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참가 물질

5

반응물 3

HCID 7672Phenyl isocyanateHCID 8083MorpholineHCID 137410133-Chloro-4,5-dimethoxypyridazine

생성물 1

HCID 178493809HCID 178493809, 화합물수율 61.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

3-Chloro-4,5-dimethoxypyridazine (17.0 g) and morpholine (59.0 mL) were stirred at 100° C. for 2 hr, and cooled to 0° C. To the reaction mixture was added phenyl isocyanate (73.8 mL) at 0° C., and the mixture was stirred at the same temperature for 30 min, and diluted with ethyl acetate. The resulting solid was removed by filtration. The filtrate was concentrated, and the residue was purified by column chromatography (ethyl acetate/hexane-methanol/ethyl acetate) to give the title compound (9.61 g).

후처리

  1. customThe resulting solid was removed by filtration
  2. concentrationThe filtrate was concentrated
  3. customthe residue was purified by column chromatography (ethyl acetate/hexane-methanol/ethyl acetate)

출처 및 근거

ORD 기록
ord-431a0c70d78e4904b73982c60d4ce753
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09090586B2

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