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

Hydrochloric Acid → HCID 20339412、化合物

HRID 1395449
ノート
印刷プレビュー

反応式

HRID 1395449 の反応式
[F:1][C:2]([F:19])([F:18])[C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]1[CH2:13][CH2:14][NH:15][CH2:16][CH:8]1[C:7](=[O:17])[NH:6]2.[CH:20]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)=[CH2:21].CO.Cl>C(O)C.C(O)(=O)C>[N:23]1[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=1[CH2:20][CH2:21][N:15]1[CH2:14][CH2:13][N:9]2[C:10]3[C:5]([NH:6][C:7](=[O:17])[CH:8]2[CH2:16]1)=[CH:4][C:3]([C:2]([F:18])([F:1])[F:19])=[CH:12][CH:11]=3
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 75212-VinylpyridineHCID 203394142,3,4,4a-Tetrahydro-8-(trifluoromethyl)-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one

生成物 1

HCID 20339412HCID 20339412、化合物収率 71%

試薬・触媒・溶媒 2

HCID 176Acetic Acid
溶媒
HCID 702Ethanol溶媒

実験手順

A solution of 8.5 g. (0.03 mole) of 2,3,4,4a-tetrahydro-8-trifluoromethyl-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one and 17.5 g. (0.16 mole) of 2-vinylpyridine in 250 ml. of methanol containing 7 ml. acetic acid was heated under reflux for 20 hours. The reaction mixture was cooled, and the solvent was removed under reduced pressure. The residue was precipitated with 1 l. of water. The product was filtered and recrystallized from methanol-water to yield 10.1 g. of free base. 4.5 G. of this free base was dissolved in 150 ml. of absolute ethanol and treated with dry hydrogen chloride saturated ether solution. The product hydrochloride was filtered and recrystallized two times from methanol-ether to give 4 g. (71%) of the title compound as the dihydrochloride salt, m.p. 194°-196° C.

後処理

  1. temperatureunder reflux for 20 hours
  2. temperatureThe reaction mixture was cooled
  3. customthe solvent was removed under reduced pressure
  4. customThe residue was precipitated with 1 l
  5. filtrationThe product was filtered
  6. customrecrystallized from methanol-water
  7. customto yield 10.1 g
  8. dissolutionof this free base was dissolved in 150 ml
  9. filtrationThe product hydrochloride was filtered
  10. customrecrystallized two times from methanol-ether
  11. customto give 4 g

出典と根拠

ORDレコード
ord-957a35fd298a4cc28c3e29bf5720b8a3
出典データセット
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04203987

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