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Hydrochloric Acid → HCID 68870503, 화합물

HRID 2374860
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HRID 2374860 반응식
[CH3:1][S:2][C:3]1[N:4]=[N:5][C:6]([CH:9]([NH:11]C(=O)OC(C)(C)C)[CH3:10])=[CH:7][N:8]=1.[ClH:19]>CO.O1CCOCC1.C(OCC)(=O)C>[ClH:19].[CH3:1][S:2][C:3]1[N:4]=[N:5][C:6]([CH:9]([NH2:11])[CH3:10])=[CH:7][N:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 58711973HCID 58711973, 화합물2회

생성물 1

HCID 68870503HCID 68870503, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

To a stirred solution of tert-butyl 1-[3-(methylthio)-1,2,4-triazin-6-yl]ethylcarbamate (Intermediate 3) (13.3 g, 49 mmol) in methanol (100 mL) was added 4N HCl in dioxane (50 mL). After stirring for 30 minutes the volatiles were removed under reduced pressure to provide a colorless oil. The oil was taken up in ethyl acetate, and the volatiles again removed under reduced pressure to give 1-[3-(methylthio)-1,2,4-triazin-6-yl]ethanamine hydrochloride (10.1 g) as a white solid. MS m/z 171 (M+1). A portion of the white solid (90 mg) was slurried in ethyl acetate and washed with saturated sodium bicarbonate solution causing the solid to dissolve. The volatiles were removed under reduced pressure to give 1-[3-(methylthio)-1,2,4-triazin-6-yl]ethanamine (68 mg) as a foam. MS m/z 171 (M+1).

후처리

  1. customwere removed under reduced pressure
  2. customto provide a colorless oil
  3. customthe volatiles again removed under reduced pressure

출처 및 근거

ORD 기록
ord-d61e9544f56545cd831793e22671b33e
출처 데이터셋
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07462614B2

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