Dimethyl Sulfoxide → 2-Chloro-6-sulfanylbenzonitrile

HRID 869374ノート

反応式

HRID 869374 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6](Cl)[C:3]=1[C:4]#[N:5].C[S:12](C)=O>>[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([SH:12])[C:3]=1[C:4]#[N:5]

参加物

3

反応物 2

HCID 679Dimethyl SulfoxideHCID 3031Dichlobenil

生成物 1

HCID 212247652-Chloro-6-sulfanylbenzonitrile

実験手順

The solution of 2,6-dichloro-benzonitrile (20 mmol) in DMSO (dimethyl sulfoxide, 30 mL) was heated to 70° C., followed by addition of Na2S.9H2O portionwise under stirring. The mixture was stirred for 1 hour. TLC monitored the reaction. After the reaction completed, the mixture was cooled and extracted between water and ethyl acetate. The aqueous layer was acidified by hydrochloric acid to pH=3˜4 under stirring. The formed solids were collected by filtration and dried to give 2.3 g of 2-chloro-6-mercapto-benzonitrile (2A). MS (ESI): M++1=170.6.

後処理

  1. stirringThe mixture was stirred for 1 hour
  2. customthe reaction
  3. temperaturethe mixture was cooled
  4. extractionextracted between water and ethyl acetate
  5. stirringunder stirring
  6. filtrationThe formed solids were collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-1fa06ab57c4b4f6690ceda09a4b7aa5c
出典データセット
uspto-grants-2015_03
特許番号
US08969373B2

反応ノート

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