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Hydrochloric Acid → HCID 10219783、化合物

HRID 650114
ノート
印刷プレビュー

反応式

HRID 650114 の反応式
[C:1]([NH:5][C:6](=[O:17])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[O:13]C(=O)C)([CH3:4])([CH3:3])[CH3:2].O.Cl>C1COCC1>[C:1]([NH:5][C:6](=[O:17])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[OH:13])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 962WaterHCID 1279601HCID 1279601、化合物

生成物 1

HCID 10219783HCID 10219783、化合物収率 80.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The product from Step A (2.35 g, 0.010 mol) was dissolved in THF wand 10 mL of water was added to form a clear suspension. Hydrochloric acid (5%) was added until the solution reached a pH˜1. The reaction mixture was then refluxed for 24 hours. TLC indicated that about half of the starting material remained, so an additonal 10 mL of 5% hydrochloric acid was added and the reaction mixture was refluxed for 24 hours. The THF was then removed by rotoevaporation and the remaining aqueous mixture was extracted with hexanes (2×20 mL). The combined hexane layers were washed with water (2×40 mL), dried over MgSO4 and the hexane removed in vacuo to provide 1.56 g (80.8% yield) of the title compound as a white crystalline solid, m.p. 78-79.5° C.

後処理

  1. additionwas added
  2. customto form a clear suspension
  3. temperatureThe reaction mixture was then refluxed for 24 hours
  4. additionwas added
  5. temperaturethe reaction mixture was refluxed for 24 hours
  6. customThe THF was then removed by rotoevaporation
  7. extractionthe remaining aqueous mixture was extracted with hexanes (2×20 mL)
  8. washThe combined hexane layers were washed with water (2×40 mL)
  9. dry with materialdried over MgSO4
  10. customthe hexane removed in vacuo

出典と根拠

ORDレコード
ord-0693be00f88a48e58e7d7636c98dab9e
出典データセット
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06271265B1

反応ノート

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