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Sodium Hydroxide → HCID 59514534, 화합물

HRID 1159680
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HRID 1159680 반응식
[CH2:1]([O:8][C:9]([NH:11][C:12]1[CH:32]=[CH:31][C:15]([CH2:16][C:17]2[N:22]=[C:21]([N:23]([CH3:25])[CH3:24])[C:20]([CH2:26][C:27]([O:29]C)=[O:28])=[CH:19][N:18]=2)=[CH:14][CH:13]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>O1CCCC1.CO>[CH2:1]([O:8][C:9]([NH:11][C:12]1[CH:13]=[CH:14][C:15]([CH2:16][C:17]2[N:22]=[C:21]([N:23]([CH3:24])[CH3:25])[C:20]([CH2:26][C:27]([OH:29])=[O:28])=[CH:19][N:18]=2)=[CH:31][CH:32]=1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 59514555HCID 59514555, 화합물

생성물 1

HCID 59514534HCID 59514534, 화합물수율 78%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of methyl [2-(4-{[(benzyloxy)carbonyl]amino}benzyl)-4-(dimethylamino)pyrimidin-5-yl]acetate (1.51 g, 3.48 mmol) in tetrahydrofuran (8 mL) and methanol (15 mL) was added 1N NaOH aq. (5 mL). The reaction mixture was stirred for 20 hours at room temperature and concentrated under reduced pressure. The residue was neutralized with 1N hydrochloric acid and concentrated under reduced pressure. This residue was dissolved with chloroform/methanol (10:1) and the insolubles were removed by filtration. The filtrate was concentrated under reduced pressure. The residual solid was recrystallized with acetonitrile/ethanol (10:1) to give [2-(4-{[(benzyloxy)carbonyl]amino}benzyl)-4-(dimethylamino)pyrimidin-5-yl]acetic acid (1.14 g, 78%) as a white solid.

후처리

  1. concentrationconcentrated under reduced pressure
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThis residue was dissolved with chloroform/methanol (10:1)
  4. customthe insolubles were removed by filtration
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customThe residual solid was recrystallized with acetonitrile/ethanol (10:1)

출처 및 근거

ORD 기록
ord-8747c60a8d9d40df9c6bdf80a6badd68
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07812160B2

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