Triacetoxyperiodinane → HCID 86645365、化合物

HRID 1959614ノート

反応式

HRID 1959614 の反応式
CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.[Cl:23][C:24]1[CH:29]=[CH:28][N:27]=[C:26]([CH2:30][OH:31])[C:25]=1[CH2:32][O:33][CH:34]1[CH2:39][CH2:38][CH2:37][CH2:36][O:35]1>C1COCC1>[Cl:23][C:24]1[CH:29]=[CH:28][N:27]=[C:26]([CH:30]=[O:31])[C:25]=1[CH2:32][O:33][CH:34]1[CH2:39][CH2:38][CH2:37][CH2:36][O:35]1

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 67077239HCID 67077239、化合物

生成物 1

HCID 86645365HCID 86645365、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Dess-Martin periodinane (370 mg. 0.873 mmol) was added to a stirred solution of [4-chloro-3-(tetrahydro-pyran-2-yloxymethyl)-pyridin-2-yl]-methanol (150 mg. 0.582 mmol) in THF (5 mL). After stirring for 2 h at room temperature the reaction was concentrated. Sat. NaHCO3 solution (20 mL) was added and extracted three times with DCM (50 mL). The combined organic layers were dried over Na2SO4 filtered and concentrated in vacuo. The resulting title compound was used for the next reaction without purification. MS (m/z): 255.7 [M+H+].

後処理

  1. concentrationwas concentrated
  2. additionSat. NaHCO3 solution (20 mL) was added
  3. extractionextracted three times with DCM (50 mL)
  4. dry with materialThe combined organic layers were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe resulting title compound was used for the next reaction without purification

出典と根拠

ORDレコード
ord-f34771091b8047cdbc4552c352c45dfc
出典データセット
uspto-grants-2013_04
特許番号
US08410134B2

反応ノート

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