Hydrochloric Acid → 2-Heptyloxy-4-iodobenzaldehyde

HRID 1171442

反応式

HRID 1171442 の反応式
CS(C)=O.C(Cl)(=O)C(Cl)=O.[CH2:11]([O:18][C:19]1[CH:24]=[C:23]([I:25])[CH:22]=[CH:21][C:20]=1[CH2:26][OH:27])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].Cl>ClCCl>[CH2:11]([O:18][C:19]1[CH:24]=[C:23]([I:25])[CH:22]=[CH:21][C:20]=1[CH:26]=[O:27])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 679Dimethyl SulfoxideHCID 65578Oxalyl chlorideHCID 68768142(2-Heptyloxy-4-iodophenyl)methanol

生成物 1

HCID 860544942-Heptyloxy-4-iodobenzaldehyde

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

A solution of dimethyl sulfoxide (3 ml, 41.4 mmol) in dichloromethane is added to a solution of oxalyl chloride (20.7 mmol, 1.8 ml) in dichloromethane (55 ml). A solution of (2-heptyloxy-4-iodophenyl)methanol (6.55 g, 18.8 mmol) in 25 ml of dichloromethane is added dropwise to the solution previously obtained, at −78° C. The mixture is stirred until the temperature returns to room temperature. The organic phase is acidified with a 2N hydrochloric acid solution. The desired product is extracted by addition of ethyl acetate. The organic phase is washed with water, dried with magnesium sulfate and concentrated using a rotary evaporator. 6.5 g (100%) of the expected compound are recovered in the form of a yellow solid.

後処理

  1. custompreviously obtained, at −78° C
  2. extractionThe desired product is extracted by addition of ethyl acetate
  3. washThe organic phase is washed with water
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated
  6. customa rotary evaporator
  7. custom6.5 g (100%) of the expected compound are recovered in the form of a yellow solid

出典と根拠

ORDレコード
ord-cb547eed9e454edfb53e66fa6ab30b5e
出典データセット
uspto-grants-2010_11
特許番号
US07829588B2

関連ノート

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