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Hydrochloric Acid → 7-(2-Fluoro-4-iodo-phenylamino)-pyrrolo[1,2-c]pyrimidine-6-carboxylic acid

HRID 450116
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HRID 450116 반응식
C([O:3][C:4]([C:6]1[CH:7]=[C:8]2[CH:13]=[CH:12][N:11]=[CH:10][N:9]2[C:14]=1[NH:15][C:16]1[CH:21]=[CH:20][C:19]([I:22])=[CH:18][C:17]=1[F:23])=[O:5])C.O.[OH-].[Li+].Cl>O1CCOCC1.O>[F:23][C:17]1[CH:18]=[C:19]([I:22])[CH:20]=[CH:21][C:16]=1[NH:15][C:14]1[N:9]2[CH:10]=[N:11][CH:12]=[CH:13][C:8]2=[CH:7][C:6]=1[C:4]([OH:5])=[O:3]
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 672343197-(2-Fluoro-4-iodo-phenylamino)-pyrrolo[1,2-c]pyrimidine-6-carboxylic acid ethyl ester

생성물 1

HCID 672358207-(2-Fluoro-4-iodo-phenylamino)-pyrrolo[1,2-c]pyrimidine-6-carboxylic acid

시약·촉매·용매 2

HCID 962Water용매
HCID 31275
1,4-Dioxane
용매

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온도
60 °C

실험 절차

To a solution of 7-(2-fluoro-4-iodo-phenylamino)-pyrrolo[1,2-c]pyrimidine-6-carboxylic acid ethyl ester (230 mg, 0.54 mmol) in a mixture of dioxane (2 mL) and water (1 mL) was added lithium hydroxide monohydrate (45 mg, 1.08 mmol). The reaction was heated at 60° C. for 1 hour. Aqueous hydrochloric acid (1M) was added dropwise until pH˜5 causing a precipitate to form. The reaction mixture was filtered and the solid residue washed with ethyl acetate (5 mL) to yield the title compound as an off white solid (67 mg, 31%). LCMS (Method B): RT=3.22 min, M+H+=398.

후처리

  1. customto form
  2. filtrationThe reaction mixture was filtered
  3. washthe solid residue washed with ethyl acetate (5 mL)

출처 및 근거

ORD 기록
ord-8ffbcf5384124647bde7fa0b5364d5bf
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486963B2

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