Sulfuric Acid → HCID 178501284, 화합물

HRID 1516150노트

반응식

HRID 1516150 반응식
[OH:1][C@@H:2]1[CH2:7][CH2:6][C@H:5]([C:8]([OH:10])=[O:9])[CH2:4][CH2:3]1.S(=O)(=O)(O)O.[C:16](=O)([O-])[O-].[Na+].[Na+]>CO>[CH3:16][O:9][C:8]([C@H:5]1[CH2:6][CH2:7][C@@H:2]([OH:1])[CH2:3][CH2:4]1)=[O:10]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 178525779HCID 178525779, 화합물

생성물 1

HCID 178501284HCID 178501284, 화합물수율 94%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of cis-4-hydroxy-cyclohexanecarboxylic acid (10.0 g, 69.4 mmol) and a catalytic amount of concentrated sulfuric acid in methanol (700 ml) was heated at reflux over night. After cooling to room temperature the reaction mixture was neutralized by the addition of solid sodium carbonate. The mixture was stirred for 30 min, filtered and concentrated in vacuo. The residue was triturated in ethyl acetate (150 ml). The solids were removed by filtration. The filtrate was concentrated in vacuo to give the crude product (10.3 g, 94%) as colorless oil, which was used in the following steps without further purification. MS m/e: 159 (M+H+).

후처리

  1. temperatureat reflux over night
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. customThe residue was triturated in ethyl acetate (150 ml)
  5. customThe solids were removed by filtration
  6. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-e928e8f2d5ef4a72b80aa567dde9d2fe
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08227458B2

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