Diethyl Ether → 4-[2-[(E)-2-iodovinyl]-phenoxy]-butan-1-ol

HRID 2081320노트

반응식

HRID 2081320 반응식
C([O:3][C:4](=O)[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1/[CH:15]=[CH:16]/[I:17])C.[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)C>O1CCCC1>[I:17]/[CH:16]=[CH:15]/[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[O:8][CH2:7][CH2:6][CH2:5][CH2:4][OH:3]

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 150701204-[2-[(E)-2-iodovinyl]-phenoxy]butyric acid ethyl esterHCID 21226445Aluminium lithium hydride

생성물 1

HCID 150701424-[2-[(E)-2-iodovinyl]-phenoxy]-butan-1-ol수율 54.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 250 mg of 4-[2-[(E)-2-iodovinyl]-phenoxy]butyric acid ethyl ester in 5 ml of tetrahydrofuran is instilled into a suspension of 80 mg of lithium aluminum hydride at 0° C. with stirring and under argon atmosphere. Then, it is stirred for an hour with ice cooling, the mixture is decomposed under argon atmosphere with ice water, shaken out with diethyl ether, dried (Na2SO4) and concentrated by evaporation. 120 mg of 4-[2-[(E)-2-iodovinyl]-phenoxy]-butan-1-ol is obtained as a yellow oil, which is further reacted as a crude product.

후처리

  1. stirringThen, it is stirred for an hour with ice cooling
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-042a509286504dbda294c99e3f1377be
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05183925

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