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

Dimethylamine → 1,1-dimethylethyl [5-[(N,N-dimethylglycyl)(methyl)amino]-2-(methyloxy)phenyl]carbamate

HRID 1014390
ノート
印刷プレビュー

反応式

HRID 1014390 の反応式
[CH3:1][NH:2][C:3]1[CH:4]=[CH:5][C:6]([O:17][CH3:18])=[C:7]([NH:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[CH:8]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:26][C:27](Cl)=[O:28].[CH3:30][NH:31][CH3:32].C(=O)(O)[O-].[Na+].C(OCC)(=O)C>O1CCCC1>[CH3:30][N:31]([CH3:32])[CH2:26][C:27]([N:2]([CH3:1])[C:3]1[CH:4]=[CH:5][C:6]([O:17][CH3:18])=[C:7]([NH:9][C:10](=[O:16])[O:11][C:12]([CH3:14])([CH3:15])[CH3:13])[CH:8]=1)=[O:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 674DimethylamineHCID 11430Potassium CarbonateHCID 89602Bromoacetyl chlorideHCID 594418351,1-Dimethylethyl [5-(methylamino)-2-(methyloxy)phenyl]carbamateHCID 86584982Sodium bicarbonate ethyl acetate

生成物 1

HCID 594420081,1-dimethylethyl [5-[(N,N-dimethylglycyl)(methyl)amino]-2-(methyloxy)phenyl]carbamate
収率 78%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A suspension of 1,1-dimethylethyl [5-(methylamino)-2-(methyloxy)phenyl]carbamate (2.15 g, 8.52 mmol) and potassium carbonate (2.355 g, 17.04 mmol) in tetrahydrofuran (75 ml) was treated with bromoacetylchioride (0.779 ml, 9.37 mmol), stirred for 45 minutes, and dimethyl amine in THF (17.04 ml, 34.1 mmol) was added. The solution was stirred at room temperature for 8 hours, poured into saturated sodium bicarbonate/ethyl acetate, and the organic layer was separated, dried over sodium sulfate, filtered, taken to a residue under reduced pressure, and purified by column chromatography to afford 1,1-dimethylethyl [5-[(N,N-dimethylglycyl)(methyl)amino]-2-(methyloxy)phenyl]carbamate (2.25 g, 6.67 mmol, 78% yield) as a yellow oil. 1H NMR (400 MHz, DMSO-d6) δ ppm 8.05 (br. s., 1 H), 7.60 (br. s., 1 H), 6.88-7.10 (m, 2 H), 3.82 (s, 3 H), 3.08 (s, 3 H), 2.80 (br. s., 2 H), 2.11 (s, 6 H), 1.36-1.54 (m, 9 H)

後処理

  1. stirringThe solution was stirred at room temperature for 8 hours
  2. customthe organic layer was separated
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. custompurified by column chromatography

出典と根拠

ORDレコード
ord-8ea5326844d44cda91fc222f99d3ee84
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07981903B2

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