Hydrochloric Acid → HCID 20194902, 화합물

HRID 653512노트

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HRID 653512 반응식
[CH3:1][O:2][CH:3]1[O:8][CH2:7][C:6]([C:13]([O:15]C)=[O:14])([C:9]([O:11]C)=[O:10])[CH2:5][CH2:4]1.[OH-].[Na+].Cl>O>[CH3:1][O:2][CH:3]1[O:8][CH2:7][C:6]([C:9]([OH:11])=[O:10])([C:13]([OH:15])=[O:14])[CH2:5][CH2:4]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 20194899HCID 20194899, 화합물

생성물 1

HCID 20194902HCID 20194902, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
90 °C

실험 절차

Dimethyl 6-methoxytetrahydropyran-3,3-dicarboxylate (6.6 g, 0.028 mol) was added to a solution of sodium hydroxide (2.8 g, 0.07 mol) in water (10 ml), and the mixture was heated at 90° C. for 3 hours. After the reaction mixture was cooled to 0° C., 6N hydrochloric acid (12 ml, 0.07 mol) was added to neutralize the solution. After salting out, the mixture was extracted with five 30 ml portions of ethyl ether. The combined ether extracts were dried over anhydrous magnesium sulfate, filtered, and subjected to rotary evaporation. The residual white powder was recystallized from a mixture of diethyl ether and acetone (3:1). Yield of the product, which decomposed at 136° to 140° C., was 94%.

후처리

  1. temperatureAfter the reaction mixture was cooled to 0° C.
  2. extractionthe mixture was extracted with five 30 ml portions of ethyl ether
  3. dry with materialThe combined ether extracts were dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customsubjected to rotary evaporation
  6. additionThe residual white powder was recystallized from a mixture of diethyl ether and acetone (3:1)
  7. customdecomposed at 136° to 140° C.

출처 및 근거

ORD 기록
ord-c6a894a420f34fe29a2761affca6e1a2
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04677190

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