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

Sodium Carbonate → 2-[[(4-ethoxy-3-methyl-2-pyridyl)methyl]thio]5,7-dihydro-5,5,7,7-tetramethylindeno[5,6-d]imidazol-6(1H)-one

HRID 703156
ノート
印刷プレビュー

反応式

HRID 703156 の反応式
[CH3:1][CH2:2][O-:3].[Na+].C(=O)([O-])[O-].[Na+].[Na+].[CH3:11][C:12]1([CH3:39])[C:23]2[C:15](=[CH:16][C:17]3[NH:18][C:19]([S:24][CH2:25][C:26]4[C:31]([CH3:32])=[C:30]([N+]([O-])=O)[CH:29]=[CH:28][N:27]=4)=[N:20][C:21]=3[CH:22]=2)[C:14]([CH3:37])([CH3:36])[C:13]1=[O:38]>C(O)C>[CH2:2]([O:3][C:30]1[CH:29]=[CH:28][N:27]=[C:26]([CH2:25][S:24][C:19]2[NH:18][C:17]3[CH:16]=[C:15]4[C:23](=[CH:22][C:21]=3[N:20]=2)[C:12]([CH3:11])([CH3:39])[C:13](=[O:38])[C:14]4([CH3:37])[CH3:36])[C:31]=1[CH3:32])[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 2723922Sodium ethoxideHCID 221514395,7-dihydro-5,5,7,7-tetramethyl-2-[[(3-methyl-4-nitro-2-pyridyl)methyl]thio]indeno[5,6-d]imidazol-6(1H)-one

生成物 1

HCID 221514652-[[(4-ethoxy-3-methyl-2-pyridyl)methyl]thio]5,7-dihydro-5,5,7,7-tetramethylindeno[5,6-d]imidazol-6(1H)-one

試薬・触媒・溶媒 1

HCID 702Ethanol
溶媒

実験手順

A mixture of 10.5 g of sodium ethylate. 20 g of sodium carbonate and 400 ml of ethanol was stirred at 50° under argon for 30 minutes and then treated with 7 g of 5,7-dihydro-5,5,7,7-tetramethyl-2-[[(3-methyl-4-nitro-2-pyridyl)methyl]thio]indeno[5,6-d]imidazol-6(lH)-one. After stirring at 50° for 5 hours under argon the reaction mixture was concentrated in vacuo. The residue was treated with methylene chloride and buffered by means of glacial acetic acid; the methylene chloride solution was extracted with sodium bicarbonate solution, dried and concentrated. The residue was chromatographed on silica gel while eluting with methylene chloride/ethyl acetate (3:1), the medium pressure flash chromatography method being used and the pressure being produced with nitrogen gas. There was obtained 2-[[(4-ethoxy-3-methyl-2-pyridyl)methyl]thio]5,7-dihydro-5,5,7,7-tetramethylindeno[5,6-d]imidazol-6(lH)-one which melts at 175-176° after recrystallization from ether.

後処理

  1. concentrationwas concentrated in vacuo
  2. additionThe residue was treated with methylene chloride
  3. extractionthe methylene chloride solution was extracted with sodium bicarbonate solution
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel
  7. washwhile eluting with methylene chloride/ethyl acetate (3:1)
  8. customthe pressure being produced with nitrogen gas

出典と根拠

ORDレコード
ord-1af94b54578d4df2997014bd9e9b50f5
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04981861

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