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 → 2-[[2-(3-Butoxy-phenyl)-ethyl]-(tetrahydrofuran-3-ylmethyl)amino]-N,N-dimethyl-acetamide hydrochloride

HRID 2264666
ノート
印刷プレビュー

反応式

HRID 2264666 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH2:8][CH2:9][N:10]([CH2:17][CH:18]2[CH2:22][CH2:21][O:20][CH2:19]2)[CH2:11][C:12]([N:14]([CH3:16])[CH3:15])=[O:13])[CH:5]=[CH:6][CH:7]=1.Br[CH2:24][CH2:25][CH2:26][CH3:27].C(=O)([O-])[O-].[K+].[K+].[I].[K].[ClH:36]>CN(C=O)C.CCOC(C)=O.C(OCC)C>[ClH:36].[CH2:24]([O:1][C:2]1[CH:3]=[C:4]([CH2:8][CH2:9][N:10]([CH2:17][CH:18]2[CH2:22][CH2:21][O:20][CH2:19]2)[CH2:11][C:12]([N:14]([CH3:16])[CH3:15])=[O:13])[CH:5]=[CH:6][CH:7]=1)[CH2:25][CH2:26][CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 8002Butyl bromideHCID 11430Potassium CarbonateHCID 595968312-[[2-(3-hydroxy-phenyl)-ethyl]-(tetrahydrofuran-3-ylmethyl)amino]-N,N-dimethyl-acetamideHCID 178506587HCID 178506587、化合物

生成物 1

HCID 665912022-[[2-(3-Butoxy-phenyl)-ethyl]-(tetrahydrofuran-3-ylmethyl)amino]-N,N-dimethyl-acetamide hydrochloride
収率 50%

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 2-[[2-(3-hydroxy-phenyl)-ethyl]-(tetrahydrofuran-3-ylmethyl)amino]-N,N-dimethyl-acetamide (1.0 g 3.3 mmol), 1-bromobutane (0.43 ml, 4 mmol), potassium carbonate (680 mg 5 mmol), potassium iodine (50 mg, 0.3 mmol), in DMF (30 ml) was refluxed for 16 h. After filtration over celite pad, the solution was evaporated from the solvent and the crude oil obtained purified by preparative HPLC. The hydrochloride salt was prepared by adding HCl 1N in AcOEt to the free amine dissolved in ethyl ether. After filtration, 690 mg (50% yield) the title compound was obtained as a white solid of 99% purity.

後処理

  1. filtrationAfter filtration over celite pad
  2. customthe solution was evaporated from the solvent
  3. customthe crude oil obtained
  4. custompurified by preparative HPLC
  5. filtrationAfter filtration

出典と根拠

ORDレコード
ord-8885e7c0d9a8486eac642bb50d8f14f1
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07855227B2

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