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Sodium Hydroxide → HCID 59596464, 화합물

HRID 2264960
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HRID 2264960 반응식
C(O[C:4]([C:6]1[N:14]([CH3:15])[C:13]2[CH:12]=[CH:11][N:10]=[C:9](CC)[C:8]=2[C:7]=1[NH:18][C:19]1[CH:24]=[CH:23][C:22]([I:25])=[CH:21][C:20]=1[F:26])=[O:5])C.[OH-].[Na+].[CH:29]([O:31][CH2:32][CH2:33][O:34][NH2:35])=[CH2:30].CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C>C1COCC1.CO>[CH:29]([O:31][CH2:32][CH2:33][O:34][NH:35][C:4]([C:6]1[N:14]([CH3:15])[C:13]2[CH:12]=[CH:11][N:10]=[CH:9][C:8]=2[C:7]=1[NH:18][C:19]1[CH:24]=[CH:23][C:22]([I:25])=[CH:21][C:20]=1[F:26])=[O:5])=[CH2:30]
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참가 물질

9

반응물 6

HCID 14798Sodium HydroxideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 21867017O-(2-(Vinyloxy)ethyl)hydroxylamineHCID 67212327HCID 67212327, 화합물

생성물 1

HCID 59596464
HCID 59596464, 화합물
수율 57%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

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온도
65 °C

실험 절차

A mixture of ethyl 3-(2-fluoro-4-iodo-phenylamino)-1-methyl-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester (100 mg, 0.23 mmol), 1N aqueous sodium hydroxide (0.25 ml) and MeOH (3.0 ml) was heated at 65° C. for 1.5 hours. The reaction mixture was concentrated and azeotroped with toluene (2×2 ml) to give a solid residue. The solid residue was dissolved in anhydrous THF (4 ml) and O-(2-vinyloxy-ethyl)-hydroxylamine (47 mg, 0.46 mmol), EDCI (55 mg, 0.29 mmol), HOBt (43 mg, 0.32 mmol) and DIPEA (119 μl, 0.68 mmol) were added. After stirring for 72 hours at ambient temperature, the mixture was evaporated and the residue was partitioned between ethyl acetate (30 ml) and water (20 ml). The organic layer was isolated, dried over sodium sulphate, then filtered and evaporated to give a yellow oil. The oil was purified by flash chromatography (Si-PPC, dichloromethane:methanol, gradient 100:0 to 90:10) to afford the title compound as a yellow solid (64 mg, 57%). LCMS (method B): RT=2.20 min, M+H+=497.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customazeotroped with toluene (2×2 ml)
  3. customto give a solid residue
  4. customthe mixture was evaporated
  5. customthe residue was partitioned between ethyl acetate (30 ml) and water (20 ml)
  6. customThe organic layer was isolated
  7. dry with materialdried over sodium sulphate
  8. filtrationfiltered
  9. customevaporated
  10. customto give a yellow oil
  11. customThe oil was purified by flash chromatography (Si-PPC, dichloromethane:methanol, gradient 100:0 to 90:10)

출처 및 근거

ORD 기록
ord-7c0f11d6811049da82a97cc7130e6484
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07855216B2

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