Benzene, 1,3-diiodo- → 3-(3-Iodophenyl)-3-oxetanol

HRID 334050

反応式

HRID 334050 の反応式
C([Li])CCC.I[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([I:13])[CH:8]=1.[O:14]1[CH2:17][C:16](=[O:18])[CH2:15]1.[NH4+].[Cl-]>C1COCC1>[I:13][C:9]1[CH:8]=[C:7]([C:16]2([OH:18])[CH2:17][O:14][CH2:15]2)[CH:12]=[CH:11][CH:10]=1

参加物

6

反応物 4

HCID 12270Benzene, 1,3-diiodo-HCID 25517Ammonium ChlorideHCID 150242543-OxetanoneHCID 178418339Butyllithium

生成物 1

HCID 866882783-(3-Iodophenyl)-3-oxetanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2.55 mL (6.37 mmol) n-butyl lithium (2.5 M in THF) was added dropwise to a mixture of 2.00 g (6.06 mmol) 1,3-diiodobenzene in 40 mL THF under argon atmosphere at −70° C. The resulting mixture was stirred for 15 min 476 μL (7.28 mmol) 3-oxetanone was added and the mixture was stirred over night at RT. The mixture was worked up by adding saturated NH4Cl solution followed by extraction with EtOAc. The combined organic phases were dried over magnesium sulfate, filtered and concentrated in vacuo. The crude material was purified by HPLC.

後処理

  1. additionwas added
  2. extractionfollowed by extraction with EtOAc
  3. dry with materialThe combined organic phases were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by HPLC

出典と根拠

ORDレコード
ord-318a8a5cad21415f8162d4a86d0ffd30
出典データセット
uspto-grants-2014_11
特許番号
US08883789B2

関連ノート

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