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Sodium hydride → tert-butyl 5-methoxycarbonylmethyl-1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indole-2-carboxylate

HRID 1677028
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HRID 1677028 반응식
[C:1]([N:8]1[CH2:20][CH2:19][C:11]2[NH:12][C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=3[C:10]=2[CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[H-].[Na+].Br[CH2:24][C:25]([O:27][CH3:28])=[O:26]>CN(C=O)C>[CH3:28][O:27][C:25]([CH2:24][N:12]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=2[C:10]2[CH2:9][N:8]([C:1]([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2])[CH2:20][CH2:19][C:11]1=2)=[O:26]
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참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 60984Methyl bromoacetateHCID 46344376tert-Butyl 1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indole-2-carboxylate

생성물 1

HCID 57681625tert-butyl 5-methoxycarbonylmethyl-1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indole-2-carboxylate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

N-boc-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]indole (450 mg, 1.65 mmol) was dissolved in DMF (7 mL) and stirred at room temperature. The vessel was flushed with argon and sodium hydride (67.0 mg, 1.65 mmol) was added. After 30 minutes, methyl bromoacetate (253 mg, 1.65 mmol) in DMF (2 mL) was added and the mixture stirred overnight. The solvent was removed in vacuo and the residue partitioned between brine (20 mL) and ethyl acetate (2×40 mL). Combined organics were dried (sodium sulphate), concentrated in vacuo and adsorbed onto silica for purification by flash chromatography (0-40% ethyl acetate/isohexane). This gave tert-butyl 5-methoxycarbonylmethyl-1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indole-2-carboxylate as a pale yellow foam (387 mg, 68%).

후처리

  1. additionwas added
  2. stirringthe mixture stirred overnight
  3. customThe solvent was removed in vacuo
  4. customthe residue partitioned between brine (20 mL) and ethyl acetate (2×40 mL)
  5. dry with materialCombined organics were dried (sodium sulphate)
  6. concentrationconcentrated in vacuo
  7. customadsorbed onto silica for purification by flash chromatography (0-40% ethyl acetate/isohexane)

출처 및 근거

ORD 기록
ord-43f7852d089b48d6af25f42da8975aec
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08008279B2

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