Methanol → HCID 69418093, 화합물

HRID 1375087노트

반응식

HRID 1375087 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([CH2:14][C:15]([OH:17])=[O:16])[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[CH3:18]O>S(=O)(=O)(O)O>[CH3:18][O:16][C:15](=[O:17])[CH2:14][C:8]1([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[CH2:9][CH2:10][O:11][CH2:12][CH2:13]1

참가 물질

4

반응물 2

HCID 887MethanolHCID 210779472-(4-(4-Chlorophenyl)tetrahydro-2H-pyran-4-yl)acetic acid

생성물 1

HCID 69418093HCID 69418093, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

A stirred solution of (4-{4-chloro-phenyl}-tetrahydro-pyran-4-yl)-acetic acid [3.3 g, Reference Example 21(a)] in anhydrous methanol (125 mL), under argon, was treated with concentrated sulfuric acid (8 drops). This mixture was stirred at reflux temperature for 5.5 hours then evaporated. The residue was treated with ethyl acetate (35 mL) and the resulting solution was washed three times with water (10 mL), then dried over magnesium sulfate and then evaporated to give the title compound (3.12 g) as a pale amber oil. LC-MS: RT=3.43 minutes, MS(ES+): 269 and 271(M+H)+.

후처리

  1. temperatureat reflux temperature for 5.5 hours
  2. customthen evaporated
  3. additionThe residue was treated with ethyl acetate (35 mL)
  4. washthe resulting solution was washed three times with water (10 mL)
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

출처 및 근거

ORD 기록
ord-006855bb233c4a5bbfac880e371c0697
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07166616B2

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