Hydrochloric Acid → HCID 23459800、化合物

HRID 2287202ノート

反応式

HRID 2287202 の反応式
[OH:1][C:2]1[C:15]2[C:14](=[O:16])[CH:13]=[C:12]([C:17]([O:19]C)=[O:18])[O:11][C:10]=2[C:9]([CH2:21][CH2:22][CH3:23])=[C:8]2[C:3]=1[C:4](=[O:24])[CH2:5][CH2:6][CH2:7]2.[I-].[Li+].Cl>[OH-].[K+].O>[OH:1][C:2]1[C:15]2[C:14](=[O:16])[CH:13]=[C:12]([C:17]([OH:19])=[O:18])[O:11][C:10]=2[C:9]([CH2:21][CH2:22][CH3:23])=[C:8]2[C:3]=1[C:4](=[O:24])[CH2:5][CH2:6][CH2:7]2

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 66321Lithium iodideHCID 23459796HCID 23459796、化合物

生成物 1

HCID 23459800HCID 23459800、化合物収率 82.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 14797Potassium Hydroxide溶媒

実験手順

The product from step (b) (200 mg; 0.61 mmole) in potassium hydroxide dried pyridine (5 ml) was heated on a steam bath with anhydrous lithium iodide (1 g; 7.5 mmole) for 1 hour. The mixture was cooled and concentrated hydrochloric acid diluted with an equal volume of water was added until the resulting suspension was at pH2. The product was extracted with ethylacetate, washed with water and dried (anhydrous sodium sulphate) to yield a red solid which was recrystallised from ethanol to give the title compound as red crystals (160 mg; 80%) mp 244° (decomposition).

後処理

  1. temperatureThe mixture was cooled
  2. additionwas added until the resulting suspension
  3. extractionThe product was extracted with ethylacetate
  4. washwashed with water
  5. dry with materialdried (anhydrous sodium sulphate)
  6. customto yield a red solid which
  7. customwas recrystallised from ethanol

出典と根拠

ORDレコード
ord-3b7dbbd16e3942ddbb3c7b5411bf698d
出典データセット
uspto-grants-1981_05
特許番号
US04269854

反応ノート

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