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Sodium Carbonate → HCID 14500626、化合物

HRID 1761582
ノート
印刷プレビュー

反応式

HRID 1761582 の反応式
[CH2:1]([N:5]1[C:9]([CH2:10][CH3:11])=[CH:8][CH:7]=[C:6]1[C:12](=O)[C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([NH2:19])[CH:14]=1)[CH2:2][CH2:3][CH3:4].[H-].[Al+3].[Li+].[H-].[H-].[H-].S([O-])([O-])(=O)=O.[Na+].[Na+].C(N1C(CC)=CC=C1[CH:45]([OH:53])C1C=CC=C(N)C=1)CCC.C([BH3-])#[N:55].[Na+].C(=O)([O-])[O-].[Na+].[Na+]>O1CCCC1.CO.C(O)(=O)C>[CH2:1]([N:5]1[C:9]([CH2:10][CH3:11])=[CH:8][CH:7]=[C:6]1[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([NH:19][C:45]([NH2:55])=[O:53])[CH:14]=1)[CH2:2][CH2:3][CH3:4]
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

10

反応物 6

HCID 10340Sodium CarbonateHCID 24436Sodium Sulfate2 回HCID 5003444Sodium cyanoborohydrideHCID 14500624HCID 14500624、化合物HCID 21226445Aluminium lithium hydrideHCID 21241933HCID 21241933、化合物

生成物 1

HCID 14500626
HCID 14500626、化合物
収率 61%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of 6.1 g (23 mmol) of 1-butyl-2-(3'-aminobenzoyl)-5-ethylpyrrole in 50 ml of anhydrous tetrahydrofuran was added dropwise, at room temperature, to a stirred suspension of 1 g (28 mmol) of lithium aluminum hydride in 100 ml of anhydrous tetrahydrofuran. The resulting mixture was refluxed for 15 minutes, cooled to 0° C. and the excess reagent sodium sulfate solution and solid anhydrous sodium sulfate. The insoluble material was separated by filtration and the filtrate evaporated in vacuo. The unstable crude alcohol thus obtained, 1-butyl-2-(3'-amino-α-hydroxybenzyl)-5-ethylpyrrole (6.1 g, 23 mmol) was dissolved in 75 ml of methanol, cooled to -10° C. and treated with 13 ml of glacial acetic acid and 2.8 g (44 mmol) of sodium cyanoborohydride. The reaction mixture was stirred at room temperature for 1 hour, poured into 200 ml of saturated sodium carbonate solution and the product extracted with ethyl acetate (4×300 ml). The combined extracts were washed with water (3×150 ml), dried and evaporated under reduced pressure. The residue was purified by column chromatography on 300 g of silica gel using hexane-acetone (95:5) as eluant, thus obtaining 3.5 mg (61%) of the title compound, 1-butyl-2-(3'-aminobenzyl)-5-ethylpyrrole, as an oil.

後処理

  1. temperatureThe resulting mixture was refluxed for 15 minutes
  2. customThe insoluble material was separated by filtration
  3. customthe filtrate evaporated in vacuo
  4. customThe unstable crude alcohol thus obtained
  5. temperaturecooled to -10° C.
  6. extractionthe product extracted with ethyl acetate (4×300 ml)
  7. washThe combined extracts were washed with water (3×150 ml)
  8. customdried
  9. customevaporated under reduced pressure
  10. customThe residue was purified by column chromatography on 300 g of silica gel

出典と根拠

ORDレコード
ord-25e8de3ad2854b9c9ada0b12d93a6cfe
出典データセット
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04826869

反応ノート

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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