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4-Amino-1-Boc-piperidine → HCID 178479359, 화합물

HRID 1881717
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HRID 1881717 반응식
I.[NH2:2][C:3]1[C:4]([C:11]([NH:13][C:14](=[NH:17])SC)=[O:12])=[N:5][C:6]([Cl:10])=[C:7]([NH2:9])[N:8]=1.[NH2:18][CH:19]1[CH2:24][CH2:23][N:22](C(OC(C)(C)C)=O)[CH2:21][CH2:20]1>CN(C=O)C.O>[ClH:10].[NH2:2][C:3]1[C:4]([C:11]([NH:13][C:14](=[NH:17])[NH:18][CH:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)=[O:12])=[N:5][C:6]([Cl:10])=[C:7]([NH2:9])[N:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 12682914-Amino-1-Boc-piperidineHCID 140329753methyl N-(3,5-diamino-6-chloropyrazine-2-carbonyl)carbamimidothioate;hydroiodide

생성물 1

HCID 178479359HCID 178479359, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

A solution of 1-(3,5-diamino-6-chloro-pyrazine-2-carbonyl)-2-methyl-isothiourea hydroiodide (7.2 g, 18.4 mmol) and 4-amino-1-Boc-piperidine (5.5 g, 27.5 mmol) in DMF (40 mL) is stirred and heated at 50° C. for 4 hours. The mixture is diluted with water (150 mL) and sonicated for 2 hours. The resulting suspension is collected by filtration and suspended in 4 M HCl in dioxane (40 mL). MeOH (20 mL) is added and the mixture is stirred at room temperature overnight and then filtered. The solid is washed with EtOH (2×10 mL) and dried to afford the title compound. [M+H]+ 313

후처리

  1. customsonicated for 2 hours
  2. filtrationThe resulting suspension is collected by filtration
  3. additionMeOH (20 mL) is added
  4. filtrationfiltered
  5. washThe solid is washed with EtOH (2×10 mL)
  6. customdried

출처 및 근거

ORD 기록
ord-7a3dfe5b6d9240a29d085dbdf46e1cc9
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318935B2

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