Hydrochloric Acid → HCID 178527939、化合物

HRID 452593ノート

反応式

HRID 452593 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([C:10]([NH:12][NH2:13])=[O:11])=[CH:7][CH:8]=2)[CH:3]=[N:2]1.[C:14](=S)=[S:15].C(N(CC)CC)C.Cl>C(O)C.O>[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([C:10]3[O:11][C:14]([SH:15])=[N:13][N:12]=3)=[CH:7][CH:8]=2)[CH:3]=[N:2]1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6348Carbon DisulfideHCID 8471TriethylamineHCID 433489731H-Indazole-5-carbohydrazide

生成物 1

HCID 178527939HCID 178527939、化合物収率 97%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A suspension of 1H-indazole-5-carbohydrazide (4.40 g, 25.0 mmol), carbon disulfide (3.76 mL, 62.5 mmol) and triethylamine (4.18 mL, 30.0 mmol) in ethanol (100 mL) was heated under reflux for 7 hr. After cooling, the reaction mixture was poured into water, and acidified with 1M hydrochloric acid. The precipitate was collected by filtration, dried and recrystallized from tetrahydrofuran to give the title compound (5.27 g, yield 97%) as colorless crystals.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 7 hr
  3. temperatureAfter cooling
  4. filtrationThe precipitate was collected by filtration
  5. customdried
  6. customrecrystallized from tetrahydrofuran

出典と根拠

ORDレコード
ord-d241b49365cd44fe94ea2c14f8cb0715
出典データセット
uspto-grants-2013_07
特許番号
US08492378B2

反応ノート

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