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Ammonium Chloride → HCID 20186417、化合物

HRID 2308942
ノート
印刷プレビュー

反応式

HRID 2308942 の反応式
[Cl-].[NH4+].[N+:3]([C:6]1[CH:7]=[CH:8][C:9]2[S:18][CH2:17][C:16]3[CH:15]=[N:14][NH:13][C:12]=3[C:10]=2[CH:11]=1)([O-])=O>O.C(O)C.[Fe]>[NH2:3][C:6]1[CH:7]=[CH:8][C:9]2[S:18][CH2:17][C:16]3[CH:15]=[N:14][NH:13][C:12]=3[C:10]=2[CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 25517Ammonium ChlorideHCID 20186437HCID 20186437、化合物

生成物 1

HCID 20186417HCID 20186417、化合物収率 65.9%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a stirred mixture of iron powder (8.53 g) and ammonium chloride (0.85 g) in water (22 ml) and ethanol (66 ml) was added portionwise 8-nitro-1,4dihydro[1]benzothiopyrano[4,3-c]pyrazole (6.6 g) under reflux over a period of 15 minutes. After being stirred for 30 minutes under reflux, the mixture was filtered and the filtrate was evaporated in vacuo. To the residue were added aqueous sodium bicarbonate and ethyl acetate and the mixture was stirred at room temperature. The resulting precipitate was collected by filtration, washed with water, and recrystallized from a mixture of tetrahydrofuran and methanol to give 8-amino-1,4-dihydro[1]benzothiopyrano[4,3-c]pyrazole (3.79 g).

後処理

  1. temperatureunder reflux over a period of 15 minutes
  2. temperatureunder reflux
  3. filtrationthe mixture was filtered
  4. customthe filtrate was evaporated in vacuo
  5. additionTo the residue were added aqueous sodium bicarbonate and ethyl acetate
  6. stirringthe mixture was stirred at room temperature
  7. filtrationThe resulting precipitate was collected by filtration
  8. washwashed with water
  9. customrecrystallized from a mixture of tetrahydrofuran and methanol

出典と根拠

ORDレコード
ord-f765b3498b114380bfa71af9b393ec36
出典データセット
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04692444

反応ノート

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