Benzyl Alcohol → HCID 68912874, 화합물

HRID 732637노트

반응식

HRID 732637 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 68912874HCID 68912874, 화합물수율 35.5%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 1140Toluene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-bfcc53a43181462bb460072059f1dc5b
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585886B2

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