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

Potassium Hydroxide → HCID 21217720、化合物

HRID 375888
ノート
印刷プレビュー

反応式

HRID 375888 の反応式
Cl.Cl[CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1.[CH2:11]([N:13]1[C:17]2=[N:18][C:19]3[C:24]([C:25]([NH:26][CH2:27][CH:28]4[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]4)=[C:16]2[CH:15]=[N:14]1)=[CH:23][C:22]([OH:34])=[CH:21][CH:20]=3)[CH3:12].[OH-].[K+]>CS(C)=O>[CH2:11]([N:13]1[C:17]2=[N:18][C:19]3[C:24]([C:25]([NH:26][CH2:27][CH:28]4[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]4)=[C:16]2[CH:15]=[N:14]1)=[CH:23][C:22]([O:34][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)=[CH:21][CH:20]=3)[CH3:12]
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 14797Potassium HydroxideHCID 77210Morpholine, 4-(2-chloroethyl)-, hydrochloride (1:1)HCID 9818690HCID 9818690、化合物

生成物 1

HCID 21217720HCID 21217720、化合物収率 14.7%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture of DMSO (6 mL), chloroethylmorpholine hydrochloride (1.23 g, 6.6 mmol), 1-ethyl-6-hydroxy-N- (cyclohexylmethyl) -1H-pyrazolo[3,4-b]quinolin-4-amine (2 g, 6.6 mmol) and KOH (1 g) was stirred at room temperature overnight. The reaction mixture was partitioned between CH2Cl2 and water and the CH2Cl2 layer was separated and evaporated. The residue was purified by column chromatography on silica gel eluting with 10% ethanol/ethyl acetate to afford the product as the free base. The free base was recrystallized from hot ethyl acetate/hexane to afford 0.425 g of 1-ethyl-6-[2-(4-morpholinyl)ethoxy]-N-(cyclohexylmethyl)-1H-pyrazolo[ 3,4-b]quinolin-4-amine, as a yellow powder, m.p. 176°-178° C.

後処理

  1. customThe reaction mixture was partitioned between CH2Cl2 and water
  2. customthe CH2Cl2 layer was separated
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel eluting with 10% ethanol/ethyl acetate
  5. customto afford the product as the free base
  6. customThe free base was recrystallized from hot ethyl acetate/hexane

出典と根拠

ORDレコード
ord-d3638bbc55b745ccb6b7a0dd6b192dee
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05488055

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