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Methyl iodide → 2-Methylamino-4,5,7,8-tetrahydro-thiazolo(4,5-d)azepine-6-carboxylic acid tert-butyl ester

HRID 400434
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HRID 400434 반응식
[H-].[Na+].[C:3]([O:7][C:8]([N:10]1[CH2:16][CH2:15][C:14]2[S:17][C:18]([NH2:20])=[N:19][C:13]=2[CH2:12][CH2:11]1)=[O:9])([CH3:6])([CH3:5])[CH3:4].[CH3:21]I>C1COCC1>[C:3]([O:7][C:8]([N:10]1[CH2:16][CH2:15][C:14]2[S:17][C:18]([NH:20][CH3:21])=[N:19][C:13]=2[CH2:12][CH2:11]1)=[O:9])([CH3:6])([CH3:4])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 84712457Tert-butyl 2-amino-4,5,7,8-tetrahydrothiazolo[5,4-d]azepine-6-carboxylate

생성물 1

HCID 866860382-Methylamino-4,5,7,8-tetrahydro-thiazolo(4,5-d)azepine-6-carboxylic acid tert-butyl ester

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

104 mg 60% sodium hydrid was added to 700 mg 2-amino-4,5,7,8-tetrahydro-thiazolo (4,5-d) azepine-6-carboxylic acid tert-butyl ester in 1.5 mL THF at 0° C. Then, 162 μL methyliodide was dropped to the mixture. The reaction was stirred over night at RT. The solvent was removed and the residue was purified by HPLC and 121 mg of the desired product was obtained.

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후처리

  1. customThe solvent was removed
  2. customthe residue was purified by HPLC

출처 및 근거

ORD 기록
ord-e8648030628a4576bac780fa383e0b1d
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08741892B2

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