Methanol → HCID 69418093、化合物

HRID 1375087ノート

反応式

HRID 1375087 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 69418093HCID 69418093、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-006855bb233c4a5bbfac880e371c0697
出典データセット
uspto-grants-2007_01
特許番号
US07166616B2

反応ノート

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