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Hydrochloric Acid → 4-(4-Iodo-phenoxymethyl)-5-methyl-furan-2-carboxylic acid

HRID 460047
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HRID 460047 반응식
C[O:2][C:3]([C:5]1[O:6][C:7]([CH3:19])=[C:8]([CH2:10][O:11][C:12]2[CH:17]=[CH:16][C:15]([I:18])=[CH:14][CH:13]=2)[CH:9]=1)=[O:4].[OH-].[Li+].Cl>O1CCCC1.O>[I:18][C:15]1[CH:16]=[CH:17][C:12]([O:11][CH2:10][C:8]2[CH:9]=[C:5]([C:3]([OH:4])=[O:2])[O:6][C:7]=2[CH3:19])=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 588241574-(4-Iodo-phenoxymethyl)-5-methyl-furan-2-carboxylic acid methyl ester

생성물 1

HCID 184446544-(4-Iodo-phenoxymethyl)-5-methyl-furan-2-carboxylic acid수율 70.4%

시약·촉매·용매 2

HCID 962Water용매2회
HCID 8028
Tetrahydrofuran
용매

실험 절차

A stirred solution of 4-(4-iodo-phenoxymethyl)-5-methyl-furan-2-carboxylic acid methyl ester (20) (2.7 g) in tetrahydrofuran (25 mL) was treated with a solution of lithium hydroxide (1.5 g) in water (2 mL). After 3 hours the reaction mixture was diluted with water and acidified to pH 2 with 1.0 M hydrochloric acid. The white precipitate was filtered off and dried in vacuo. The solid was triturated with ethyl acetate at 0° C. then collected by filtration to give compound 26 as a white solid (1.83 g). LC/MS system A: Rt=1.74 min.

후처리

  1. filtrationThe white precipitate was filtered off
  2. customdried in vacuo
  3. customThe solid was triturated with ethyl acetate at 0° C.
  4. filtrationthen collected by filtration

출처 및 근거

ORD 기록
ord-b6a33bbb62364ff3ba8207dc82816095
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07196089B2

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