ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

HCID 178526747、化合物 → 1H-pyrrolo(2,3-b)pyridin-4-amine

HRID 16402
ノート
印刷プレビュー

反応式

HRID 16402 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][N+:7]([O-])=[C:6]2[NH:11][CH:12]=[CH:13][C:5]=12)([O-])=O>C(O)(=O)C.[Fe]>[NH2:1][C:4]1[CH:9]=[CH:8][N:7]=[C:6]2[NH:11][CH:12]=[CH:13][C:5]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 178526747HCID 178526747、化合物

生成物 1

HCID 6392491H-pyrrolo(2,3-b)pyridin-4-amine

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

実験手順

9.35 g (167 mmol) of iron powder are added to a solution of 3.00 g (16.8 mmol) of 4-nitro-1H-pyrrolo[2,3-b]pyridine 7-oxide (from example (XVI) in 225 ml of acetic acid, and the mixture is heated under reflux for 2 hours. The crude mixtures of two such batches are combined and jointly worked up further. The solid is separated off and washed with 50 ml of acetic acid and 100 ml of tetrahydrofuran. Using a rotary evaporator, the filtrate is concentrated to dryness. The residue is diluted with 50 ml of water and the solution is made alkaline using 45% strength sodium hydroxide solution. Dichloromethane is then added, and the mixture is filtered off with suction through kieselguhr. The filtrate is extracted six times with in each case 100 ml of dichloromethane and the organic phase is dried over sodium sulfate and evaporated to dryness using a rotary evaporator. The residue is dried under high vacuum. For further purification, the residue is triturated with tetrahydrofuran and the solid is filtered off with suction. The filtrate is concentrated and the residue is taken up in dichloromethane, dried and concentrated.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 2 hours
  3. customThe solid is separated off
  4. washwashed with 50 ml of acetic acid and 100 ml of tetrahydrofuran
  5. customa rotary evaporator
  6. concentrationthe filtrate is concentrated to dryness
  7. additionThe residue is diluted with 50 ml of water
  8. additionDichloromethane is then added
  9. filtrationthe mixture is filtered off with suction through kieselguhr
  10. extractionThe filtrate is extracted six times with in each case 100 ml of dichloromethane
  11. dry with materialthe organic phase is dried over sodium sulfate
  12. customevaporated to dryness
  13. customa rotary evaporator
  14. customThe residue is dried under high vacuum
  15. customFor further purification
  16. customthe residue is triturated with tetrahydrofuran
  17. filtrationthe solid is filtered off with suction
  18. concentrationThe filtrate is concentrated
  19. customdried
  20. concentrationconcentrated

出典と根拠

ORDレコード
ord-524c3b350de94cd79a4733a00ce9359e
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07737153B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート