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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
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Water → [2-(2-Fluorobenzoyl)-1H-pyrrol-1-yl]-methyl-carbamic acid, ethyl ester

HRID 280132
ノート
印刷プレビュー

反応式

HRID 280132 の反応式
[C:1](=O)([O-])[O-].[Na+].[Na+].CI.[F:9][C:10]1[CH:28]=[CH:27][CH:26]=[CH:25][C:11]=1[C:12]([C:14]1[N:15]([NH:19][C:20](=[O:24])[O:21][CH2:22][CH3:23])[CH:16]=[CH:17][CH:18]=1)=[O:13].O>CN(C=O)C>[F:9][C:10]1[CH:28]=[CH:27][CH:26]=[CH:25][C:11]=1[C:12]([C:14]1[N:15]([N:19]([CH3:1])[C:20](=[O:24])[O:21][CH2:22][CH3:23])[CH:16]=[CH:17][CH:18]=1)=[O:13]
参加物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 962WaterHCID 6328Methyl iodideHCID 10340Sodium CarbonateHCID 13457759[2-(2-fluorobenzoyl)-1H-pyrrol-1-yl]carbamic acid, ethyl ester

生成物 1

HCID 13457760[2-(2-Fluorobenzoyl)-1H-pyrrol-1-yl]-methyl-carbamic acid, ethyl ester収率 99.5%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

Sodium carbonate (22.4 g, 0.21 mol), methyl iodide (30 g, 0.21 mol), and [2-(2-fluorobenzoyl)-1H-pyrrol-1-yl]-carbamic acid, ethyl ester (25.4 g, 0.09 mol) were combined in 100 ml of dry DMF with stirring at ambient temperature. After 72 hours, the mixture was poured into 800 ml of H2O and extracted with three 250 ml portions of DCM. The combined extracts were washed with H2O and brine, dried (MgSO4), filtered and evaporated to an oil. This oil was purified by HPLC (silica, DCM) to give 26 g (97%) of crystals, m.p. 64°-66°.

後処理

  1. extractionextracted with three 250 ml portions of DCM
  2. washThe combined extracts were washed with H2O and brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated to an oil
  6. customThis oil was purified by HPLC (silica, DCM)

出典と根拠

ORDレコード
ord-a170482dfe1f408797ac89ffc0b68ac1
出典データセット
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04588727

反応ノート

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