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Sodium Hydroxide → HCID 69675345, 화합물

HRID 2406410
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HRID 2406410 반응식
[OH-].[Na+].C([O:5][C:6](=[O:34])[CH:7]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])[C:8]1[C:9]([CH3:28])=[N:10][C:11]2[S:12][C:13]3[CH2:14][O:15][CH2:16][CH2:17][C:18]=3[C:19]=2[C:20]=1[C:21]1[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][CH:22]=1)C>C(O)C.O1CCCC1>[C:30]([O:29][CH:7]([C:8]1[C:9]([CH3:28])=[N:10][C:11]2[S:12][C:13]3[CH2:14][O:15][CH2:16][CH2:17][C:18]=3[C:19]=2[C:20]=1[C:21]1[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][CH:22]=1)[C:6]([OH:34])=[O:5])([CH3:33])([CH3:32])[CH3:31]
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참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 69672878HCID 69672878, 화합물

생성물 1

HCID 69675345HCID 69675345, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

Aqueous sodium hydroxide (2N, 2 mL, 4 mmol) was added to a stirred solution of tert-Butoxy-(2-methyl-4-p-tolyl-5,8-dihydro-6H-7-oxa-9-thia-1-aza-fluoren-3-yl)-acetic acid ethyl ester (66 mg, 0.15 mmol) in ethanol (2 mL) and tetrahydrofuran (2 mL) and the reaction was stirred for 2 hours at 60° C. The reaction was concentrated in vacuo until only the aqueous remained. The pH was adjusted to 2 by the addition of 2N aqueous HCl. The resulting solid was collected by filtration and purified by preparative HPLC to afford the title compound. LCMS 3.63 min, ES+/AP+ 425.1 (MH+).

후처리

  1. concentrationThe reaction was concentrated in vacuo until only the
  2. additionThe pH was adjusted to 2 by the addition of 2N aqueous HCl
  3. filtrationThe resulting solid was collected by filtration
  4. custompurified by preparative HPLC

출처 및 근거

ORD 기록
ord-dabc8de6e71640b3bc180ee948c36935
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809363B2

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