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Methanol → 2-Morpholin-4-ylmethyl-6-nitro-benzoic acid

HRID 880620
ノート
印刷プレビュー

反応式

HRID 880620 の反応式
C[O:2][C:3](=[O:20])[C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:13][N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1.[OH-].[Na+].CO.C1COCC1>O>[N:14]1([CH2:13][C:5]2[CH:6]=[CH:7][CH:8]=[C:9]([N+:10]([O-:12])=[O:11])[C:4]=2[C:3]([OH:20])=[O:2])[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1
参加物反応条件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 887MethanolHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 598410552-Morpholin-4-ylmethyl-6-nitro-benzoic acid methyl ester

生成物 1

HCID 598410692-Morpholin-4-ylmethyl-6-nitro-benzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

A solution of compound 5 (0.85 g) and NaOH (0.304 g) in a mixture of water (9 mL), methanol (5 mL), and THF (45 mL) was stirred at reflux for 24 h and concentrated to dryness. The residue was dissolved in water, and the solution was cooled to 0° C. and adjusted to pH 7 with 10% potassium hydrogen sulfate. The mixture was concentrated to dryness, the residue was treated with methanol, and filtered to remove solids. The filtrate was concentrated to yield compound 6 as a yellow solid.

後処理

  1. temperatureat reflux for 24 h
  2. concentrationconcentrated to dryness
  3. dissolutionThe residue was dissolved in water
  4. concentrationThe mixture was concentrated to dryness
  5. additionthe residue was treated with methanol
  6. filtrationfiltered
  7. customto remove solids
  8. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-5bcb9b132a4147e8ad8391e4111231e8
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993583B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート