Carbon Disulfide → HCID 178527753、化合物

HRID 31700ノート

反応式

HRID 31700 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 178527753HCID 178527753、化合物収率 56.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7c6492ab0f714737ba5ca4eb474de17d
出典データセット
uspto-grants-2008_09
特許番号
US07425634B2

反応ノート

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