Hydrochloric Acid → HCID 23459800, 화합물

HRID 2287202노트

반응식

HRID 2287202 반응식
[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

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 66321Lithium iodideHCID 23459796HCID 23459796, 화합물

생성물 1

HCID 23459800HCID 23459800, 화합물수율 82.9%

시약·촉매·용매 2

HCID 962Water용매HCID 14797Potassium Hydroxide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3b7dbbd16e3942ddbb3c7b5411bf698d
출처 데이터셋
uspto-grants-1981_05
특허 번호
US04269854

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