Sodium Sulfide → 2,3-Dihydro-5,6-dimethyl-3-thioxo-4-pyridazinecarbonitrile

HRID 2173471ノート

反応式

HRID 2173471 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([CH3:11])=[C:6]([CH3:10])[C:7]=1[C:8]#[N:9].[S-2:12].[Na+].[Na+]>C(O)(C)(C)C.CC(O)C>[CH3:10][C:6]1[C:5]([CH3:11])=[N:4][NH:3][C:2](=[S:12])[C:7]=1[C:8]#[N:9]

参加物

5

反応物 2

HCID 14804Sodium SulfideHCID 3340163-Chloro-5,6-dimethylpyridazine-4-carbonitrile

生成物 1

HCID 256489772,3-Dihydro-5,6-dimethyl-3-thioxo-4-pyridazinecarbonitrile

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 6386tert-Butanol溶媒

実験手順

A solution of 3-chloro-5,6-dimethylpyridazine-4-carbonitrile (100 mg, 0.60 mmol) and sodium sulfide was stirred in tert-butanol (2.0 mL) in a microwave reaction vial. The vial was sealed and irradiated at 100° C. for 10 minutes. LC/MS indicated product and no remaining starting material. The reaction solution was diluted with IPA (˜10 mL) and stirred at ambient temperature for about 15 minutes, then filtered. The solids on the filter were washed with IPA. The solute was concentrated in vacuo, and the resulting solid was dried overnight at 60° C. in a vacuum oven to give the product. LC/MS: RT=0.24 min., m/z=166 [M+H]+.

後処理

  1. customThe vial was sealed
  2. customirradiated at 100° C. for 10 minutes
  3. filtrationfiltered
  4. washThe solids on the filter were washed with IPA
  5. concentrationThe solute was concentrated in vacuo
  6. customthe resulting solid was dried overnight at 60° C. in a vacuum oven
  7. customto give the product

出典と根拠

ORDレコード
ord-3fae2a5ebada431f88ff1cc573fdb09b
出典データセット
uspto-grants-2015_06
特許番号
US09056875B2

反応ノート

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