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 Hydroxide → 3-(1-(3-(Thioxanthen-9-ylidene)-1-propyl)piperidin-4-yl)propionic acid acetate

HRID 1952829
ノート
印刷プレビュー

反応式

HRID 1952829 の反応式
[CH:1]1[C:14]2[C:13](=[CH:15][CH2:16][CH2:17][N:18]3[CH2:23][CH2:22][CH:21]([CH2:24][CH2:25][C:26]([O:28]CC)=[O:27])[CH2:20][CH2:19]3)[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.C(O)(=O)C([O-])=O.[OH-].[Na+]>C(O)C>[C:26]([OH:28])(=[O:27])[CH3:25].[CH:1]1[C:14]2[C:13](=[CH:15][CH2:16][CH2:17][N:18]3[CH2:19][CH2:20][CH:21]([CH2:24][CH2:25][C:26]([OH:28])=[O:27])[CH2:22][CH2:23]3)[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:6][C:5]=2[CH:4]=[CH:3][CH:2]=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 14798Sodium HydroxideHCID 3716971Hydrogen oxalateHCID 23301314Ethyl 3-(1-(3-(thioxanthen-9-ylidene)-1-propyl)piperidin-4-yl)propionate

生成物 1

HCID 702939563-(1-(3-(Thioxanthen-9-ylidene)-1-propyl)piperidin-4-yl)propionic acid acetate収率 56%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of ethyl 3-(1-(3-(thioxanthen-9-ylidene)-1-propyl)piperidin-4-yl)propionate (as the free base released from the above hydrogen oxalate; 3.71 g, 0.0088 mol), 4 N sodium hydroxide (10 ml) and 96% ethanol (70 ml) was stirred at room temperature overnight. Ethanol was evaporated in vacuo, the residue was dissolved in water (50 ml) and the aqueous solution was washed with diethyl ether (50 ml). The aqueous phase was neutralised with acetic acid and extracted with dichloromethane (3×150 ml). The combined dichloromethane extracts tracts were dried (MgSO4) and evaporated in vacuo. The residue was dissolved in acetone (30 ml), the solution was diluted with diethyl ether (30 ml) and the mixture was stirred for 1 h. The precipitated solid was filtered off, washed with acetone and dried in vacuo, affording 2.24 g (56%) of the title compound.

後処理

  1. customEthanol was evaporated in vacuo
  2. dissolutionthe residue was dissolved in water (50 ml)
  3. washthe aqueous solution was washed with diethyl ether (50 ml)
  4. extractionextracted with dichloromethane (3×150 ml)
  5. dry with materialwere dried (MgSO4)
  6. customevaporated in vacuo
  7. dissolutionThe residue was dissolved in acetone (30 ml)
  8. additionthe solution was diluted with diethyl ether (30 ml)
  9. filtrationThe precipitated solid was filtered off
  10. washwashed with acetone
  11. customdried in vacuo

出典と根拠

ORDレコード
ord-65bb4b7117894c50910dff040ea4b677
出典データセット
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06114354

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