Benzyl Alcohol → HCID 69037381, 화합물

HRID 1820761노트

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HRID 1820761 반응식
Cl.CN(C)CCCN=C=NCC.[OH:13][C:14]1[CH:22]=[CH:21][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:19][C:15]=1[C:16]([OH:18])=[O:17].[CH2:27](O)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>CN(C)C1C=CN=CC=1.C(#N)C>[CH2:27]([O:17][C:16](=[O:18])[C:15]1[CH:19]=[C:20]([S:23]([CH3:26])(=[O:25])=[O:24])[CH:21]=[CH:22][C:14]=1[OH:13])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

참가 물질

6

반응물 3

HCID 244Benzyl AlcoholHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 124227802-Hydroxy-5-(methylsulfonyl)benzoic acid

생성물 1

HCID 69037381HCID 69037381, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6342Acetonitrile용매

실험 절차

5 mmol of N-(3-dimethylaminopropyl)-N′-ethyl-carbodiimid-hydrochloride was slowly added to a stirred suspension of 5 mmol 2-hydroxy-5-methanesulfonyl-benzoic acid, 5 mmol of benzyl alcohol and 0.5 mmol of 4-dimethylaminopyridine in 10 ml acetonitrile. The mixture was stirred overnight at room temperature, concentrated and treated with 10 ml of water. A few drops of diluted hydrochloric acid were added to acidify the solution. The resulting solid was filtered and then purified by chromatography (SiO2; ethyl acetate/cyclohexane 3:7) to yield the title compound as a colorless solid. MS (m/e): 305.0 (M−H, 100%)

후처리

  1. concentrationconcentrated
  2. additiontreated with 10 ml of water
  3. additionA few drops of diluted hydrochloric acid were added
  4. filtrationThe resulting solid was filtered
  5. custompurified by chromatography (SiO2; ethyl acetate/cyclohexane 3:7)

출처 및 근거

ORD 기록
ord-8640bc17a3ab471ca4f2e743175ecaf9
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07605163B2

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