Hydrochloric Acid → 2-amino-5-(N,N-dimethylaminosulfonyl)-1,3,4-thiadiazole

HRID 127128ノート

反応式

HRID 127128 の反応式
C([NH:4][C:5]1[S:6][C:7]([S:10]([N:13]([CH3:15])[CH3:14])(=[O:12])=[O:11])=[N:8][N:9]=1)(=O)C.Cl>>[NH2:4][C:5]1[S:6][C:7]([S:10]([N:13]([CH3:15])[CH3:14])(=[O:11])=[O:12])=[N:8][N:9]=1

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 128944522-acetamido-5-(N,N-dimethylaminosulfonyl)-1,3,4-thiadiazole

生成物 1

HCID 128944532-amino-5-(N,N-dimethylaminosulfonyl)-1,3,4-thiadiazole

実験手順

2-Acetamido-5-(N,N-dimethylaminosulfonyl)-1,3,4-thiadiazole (250 grams) and concentrated hydrochloric acid (1 L) were charged into a glass reaction vessel fitted with a mechanical stirrer, reflux condenser and thermometer. This mixture was refluxed for a period of about 2 hours. It was then cooled to room temperature, filtered and the solvent stripped from the filtrate using a rotary evaporator. The solid residue was washed with 10% aqueous sodium carbonate (200 ml), air dried, then crystallized from isopropanol. These crystals were the desired product 2-amino-5-(N,N-dimethylaminosulfonyl)-1,3,4-thiadiazole and having a melting point of 188°-190° C.

後処理

  1. customfitted with a mechanical stirrer
  2. temperaturereflux condenser
  3. temperatureThis mixture was refluxed for a period of about 2 hours
  4. filtrationfiltered
  5. customa rotary evaporator
  6. washThe solid residue was washed with 10% aqueous sodium carbonate (200 ml), air
  7. customdried
  8. customcrystallized from isopropanol

出典と根拠

ORDレコード
ord-ae45236eeb9d4e91821c4aa34c037b6f
出典データセット
uspto-grants-1981_03
特許番号
US04255182

反応ノート

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