Carbon Disulfide → HCID 178527753, 화합물

HRID 1645645노트

반응식

HRID 1645645 반응식
[O:1]1[C:5]2[CH:6]=[C:7]([NH2:11])[C:8]([NH2:10])=[CH:9][C:4]=2[O:3][CH2:2]1.[C:12](=S)=[S:13]>CO>[O:1]1[C:5]2[C:4](=[CH:9][C:8]3[NH:10][C:12]([SH:13])=[N:11][C:7]=3[CH:6]=2)[O:3][CH2:2]1

참가 물질

4

반응물 2

HCID 6348Carbon DisulfideHCID 30807881,2-Diamino-4,5-methylenedioxybenzene

생성물 1

HCID 178527753HCID 178527753, 화합물수율 56.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The mixture (6.48 g) containing 1,3-benzodioxol-5,6-diamine obtained in the step (78b) above was dissolved in methanol (100 ml). To the mixture, carbon disulfide (30 ml) was added and the mixture was stirred at room temperature for one day. The reaction mixture was concentrated under reduced pressure. To the solid residue, ethyl acetate was added and filtration was performed. The solid was washed by adding tetrahydrofuran, ethyl acetate and diluted hydrochloric acid and insoluble substance was collected by filtration, dried under reduced pressure at room temperature for 2 hours in a desiccator to obtain the title compound (3.8 g, 56.1% from 5,6-dinitro-1,3-benzodioxol) as a brown solid.

후처리

  1. customobtained in the step (78b)
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionTo the solid residue, ethyl acetate was added
  4. filtrationfiltration
  5. washThe solid was washed
  6. additionby adding tetrahydrofuran, ethyl acetate and diluted hydrochloric acid and insoluble substance
  7. filtrationwas collected by filtration
  8. customdried under reduced pressure at room temperature for 2 hours in a desiccator

출처 및 근거

ORD 기록
ord-6ff97df675d64cb99b3d1ace0082ef82
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08124780B2

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