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

1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 2-Hydroxy-4-nitro-benzoic acid tert-butyl ester

HRID 714851
ノート
印刷プレビュー

反応式

HRID 714851 の反応式
[OH:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].C(N=C=N[CH2:19][CH2:20][CH2:21]N(C)C)C.ON1C2C=CC=C[C:29]=2N=N1.C(=O)([O-])O.[Na+]>C(O)(C)(C)C.C(N(CC)CC)C>[OH:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([O:6][C:20]([CH3:21])([CH3:29])[CH3:19])=[O:5]
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 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 692664-Nitrosalicylic acidHCID 757711-HydroxybenzotriazoleHCID 516892Sodium Bicarbonate

生成物 1

HCID 716010782-Hydroxy-4-nitro-benzoic acid tert-butyl ester収率 35.2%

試薬・触媒・溶媒 2

HCID 6386
tert-Butanol
溶媒
HCID 8471Triethylamine溶媒

実験手順

To a solution of 2-hydroxy-4-nitrobenzoic acid (5.0 g) in tert-butyl alcohol (100 mL) were added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (6.4 g), 1-hydroxybenzotriazole (3.7 g) and triethylamine (7.6 mL), and the mixture was stirred overnight at room temperature. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (2.3 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe obtained organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-0dcf3759e4894e51a8bd95d0a14d02f9
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09187453B2

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