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

p-Anisoyl chloride → HCID 131713379、化合物

HRID 1388180
ノート
印刷プレビュー

反応式

HRID 1388180 の反応式
[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].C(O)(=O)/C=C/C(O)=O.[CH3:17][N:18]1[C:22]2([CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]2)[CH:21]([NH2:28])[CH2:20][CH2:19]1.[OH-].[Na+].[C:31](Cl)(=[O:40])[C:32]1[CH:37]=[CH:36][C:35]([O:38][CH3:39])=[CH:34][CH:33]=1.C(O)(=O)/C=C/C(O)=O>C(#N)C>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[CH3:17][N:18]1[C:22]2([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]2)[CH:21]([NH:28][C:31](=[O:40])[C:32]2[CH:37]=[CH:36][C:35]([O:38][CH3:39])=[CH:34][CH:33]=2)[CH2:20][CH2:19]1.[CH3:17][N:18]1[C:22]2([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]2)[CH:21]([NH:28][C:31](=[O:40])[C:32]2[CH:37]=[CH:36][C:35]([O:38][CH3:39])=[CH:34][CH:33]=2)[CH2:20][CH2:19]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 4

HCID 7477p-Anisoyl chlorideHCID 14798Sodium HydroxideHCID 444972Fumaric AcidHCID 70447095HCID 70447095、化合物

生成物 1

HCID 131713379HCID 131713379、化合物収率 15.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a stirring suspension of 3.5 g (0.021 mole) of 1-methyl-4-amino-1-azaspiro[4.5]decane of Example 2 and 150 ml of 10% NaOH was added dropwise 3.8 g (0.022 mole) of p-anisoyl chloride. The reaction was stirred vigorously for 5 hours, the aqueous solution was decanted and the remaining oil was dissolved in ethyl acetate and dried over Na2SO4. The solvent was then evaporated to give a solid which was recrystallized from hexane to give 4.4 g. The solid was dissolved in 20 ml of acetonitrile and 1.7 g of fumaric acid was added. The suspension was stirred until the amine salt precipitated from solution. The compound was filtered and recrystallized twice from ethanol-ether to give 1.2 g (15.8%) of 1-methyl-4-(4-methoxybenzamido)-1-azaspiro[4.5]decane hemifumarate, m.p. (softens at 110° C.) 152°-155° C.

後処理

  1. customthe aqueous solution was decanted
  2. dissolutionthe remaining oil was dissolved in ethyl acetate
  3. dry with materialdried over Na2SO4
  4. customThe solvent was then evaporated
  5. customto give a solid which
  6. customwas recrystallized from hexane
  7. customto give 4.4 g
  8. customprecipitated from solution
  9. filtrationThe compound was filtered
  10. customrecrystallized twice from ethanol-ether

出典と根拠

ORDレコード
ord-b92155aae44f43dfaaa3f236a5c93a41
出典データセット
uspto-grants-1984_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04430335

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