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Hydrochloric Acid → HCID 49757564, 화합물

HRID 600285
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HRID 600285 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([NH:8]C(=O)OC(C)(C)C)=[C:4]([NH:16][CH2:17][CH2:18][O:19][CH2:20][CH2:21][CH3:22])[CH:3]=1.Cl>O1CCOCC1>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([NH2:8])=[C:4]([NH:16][CH2:17][CH2:18][O:19][CH2:20][CH2:21][CH3:22])[CH:3]=1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 45379839HCID 45379839, 화합물

생성물 1

HCID 49757564HCID 49757564, 화합물수율 100%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

A solution of tert-butyl 6-chloro-4-[(2-propoxyethyl)amino]pyridin-3-ylcarbamate (7.08 g, 21.4 mmol) in 1,4-dioxane (20 mL) was treated with 4N HCl in 1,4-dioxane (100 mL) and stirred at room temperature for one hour. The reaction was partitioned between ethyl acetate and saturated sodium bicarbonate solution. The layers were separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate, and solvent was removed at reduced pressure to give 6-chloro-N4-(2-propoxyethyl)pyridine-3,4-diamine as a brown oil. (4.93 g, 100% yield). 1H NMR (CDCl3) δ 7.63 (1H), 6.45 (1H), 4.67 (1H), 3.67 (2H), 3.43 (2H), 3.32-3.27 (2H), 2.92 (2H), 1.64-1.55 (2H), 0.93 (3H).

후처리

  1. customThe reaction was partitioned between ethyl acetate and saturated sodium bicarbonate solution
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over magnesium sulfate, and solvent
  6. customwas removed at reduced pressure

출처 및 근거

ORD 기록
ord-a39ef2b572aa47d9a8d29a14ceddee26
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07902195B2

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