Methyl Ethyl Ketone → HCID 178492798、化合物

HRID 22759

反応式

HRID 22759 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([O:8][CH3:9])=[CH:6][CH:7]=1.NC(N)=[S:12].CC(CC)=O>O>[SH:12][C:2]1[N:3]=[N:4][C:5]([O:8][CH3:9])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 6569Methyl Ethyl KetoneHCID 744033-Chloro-6-methoxypyridazineHCID 2723790Thiourea

生成物 1

HCID 178492798HCID 178492798、化合物収率 24%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3-chloro-6-methoxy pyridazine (0.69 mol, 100 g), thiourea (1.38 mol, 105 g) and ethyl methyl ketone (1.8 L) was refluxed for 3 hours. The reaction was cooled and the supernatant was poured into water and extracted with 1M sodium hydroxide (4×100 mL). The sodium hydroxide solution was washed with EtOAc (2×50 mL), the aqueous extract was acidified with sufficient conc. HCl to lower the pH to 5 and the resulting yellow solid was collected and air-dried to obtain 3-mercapto-6-methoxy pyridazine (24%, 23 g); mp 198° C.-200° C.

後処理

  1. temperaturewas refluxed for 3 hours
  2. temperatureThe reaction was cooled
  3. extractionextracted with 1M sodium hydroxide (4×100 mL)
  4. washThe sodium hydroxide solution was washed with EtOAc (2×50 mL)
  5. extractionthe aqueous extract
  6. customthe resulting yellow solid was collected
  7. customair-dried

出典と根拠

ORDレコード
ord-76473388b085410688169bdc886dcb6f
出典データセット
uspto-grants-2005_02
特許番号
US06849629B2

関連ノート

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