Benzyl Alcohol → HCID 68912874、化合物

HRID 732637ノート

反応式

HRID 732637 の反応式
[CH3:1][C:2]([CH3:15])([CH2:6][CH2:7][CH2:8][C:9]([CH3:14])([CH3:13])[C:10]([OH:12])=[O:11])[C:3]([OH:5])=[O:4].[CH2:16](O)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C1(C)C=CC(S(O)(=O)=O)=CC=1.C1(C)C=CC=CC=1>[CH2:16]([O:11][C:10](=[O:12])[C:9]([CH3:14])([CH3:13])[CH2:8][CH2:7][CH2:6][C:2]([CH3:15])([CH3:1])[C:3]([OH:5])=[O:4])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

5

反応物 2

HCID 244Benzyl AlcoholHCID 27331562,2,6,6-Tetramethylpimelic Acid

生成物 1

HCID 68912874HCID 68912874、化合物収率 35.5%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 1140Toluene溶媒

実験手順

At room temperature, 34 mg of p-toluenesulfonic acid was added to a mixture of 4.33 g of 2,2,6,6-tetramethylpimelic acid (mfd. by Tokyo Kasei (TCI), Japan), 4.24 g of benzyl alcohol and 16 ml of toluene. By equipping with a Dean-Stark type dehydration tube, this was stirred for 60Hours while heating under reflux, and then cooled down to room temperature. The insoluble matter was removed by filtration, the filtrate was concentrated under a reduced pressure, and the thus obtained residue was purified by a silica gel column chromatography (methanol-chloroform) to obtain 2.18 g of 7-(benzyloxy)-2,2,6,6-tetramethyl-7-oxoheptanoic acid as a colorless oily substance. FP: 307.

後処理

  1. temperaturewhile heating
  2. temperatureunder reflux
  3. customThe insoluble matter was removed by filtration
  4. concentrationthe filtrate was concentrated under a reduced pressure
  5. customthe thus obtained residue was purified by a silica gel column chromatography (methanol-chloroform)

出典と根拠

ORDレコード
ord-bfcc53a43181462bb460072059f1dc5b
出典データセット
uspto-grants-2009_09
特許番号
US07585886B2

反応ノート

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