HCID 59542515, 화합물 → HCID 59542565, 화합물

HRID 1809053노트

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HRID 1809053 반응식
C([O:3][C:4]([C:6]1[CH:10]=[C:9]([CH2:11][C:12]([F:15])([F:14])[F:13])[S:8][CH:7]=1)=[O:5])C>[OH-].[Na+]>[F:15][C:12]([F:13])([F:14])[CH2:11][C:9]1[S:8][CH:7]=[C:6]([C:4]([OH:5])=[O:3])[CH:10]=1

참가 물질

3

반응물 1

HCID 59542515HCID 59542515, 화합물

생성물 1

HCID 59542565HCID 59542565, 화합물수율 20.1%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

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온도
140 °C

실험 절차

5-(2,2,2-Trifluoro-ethyl)-thiophene-3-carboxylic acid ethyl ester (1.24 g, 5.2 mmol) was dissolved in IMS (10 mL) and aqueous sodium hydroxide (1 M, 10 mL) was added. The reaction was heated to 140° C. using microwave irradiation for 20 minutes and then partitioned between water and DCM. The aqueous solution was separated, acidified with 1 N hydrochloric acid and then extracted with DCM. The organic solution was dried over magnesium sulphate, filtered and the solvent removed. The resulting oil was triturated with cyclohexane and minimal diethyl ether to give the title compound (0.22 g). 1H NMR (400 MHz, CHCl3-d): δ 8.2 (s, 1H), 7.5 (s, 1H), 3.6 (q, 2H).

후처리

  1. custommicrowave irradiation for 20 minutes
  2. custompartitioned between water and DCM
  3. customThe aqueous solution was separated
  4. extractionextracted with DCM
  5. dry with materialThe organic solution was dried over magnesium sulphate
  6. filtrationfiltered
  7. customthe solvent removed
  8. customThe resulting oil was triturated with cyclohexane and minimal diethyl ether

출처 및 근거

ORD 기록
ord-57e101f96db1487d92416168d9806197
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362008B2

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