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5-Amino-2-chloropyridine → HCID 86600792, 화합물

HRID 602743
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HRID 602743 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([NH2:8])=[CH:4][CH:3]=1.[N:9]([O-])=O.[Na+].O.O.[Sn](Cl)(Cl)(Cl)Cl>Cl>[ClH:1].[Cl:1][C:2]1[N:7]=[CH:6][C:5]([NH:8][NH2:9])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 793055-Amino-2-chloropyridineHCID 23668193Sodium NitriteHCID 85782573Tin tetrachloride dihydrate

생성물 1

HCID 86600792HCID 86600792, 화합물수율 99.7%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매2회

실험 절차

To 0.5 g (3.9 mmol) of 6-chloro-pyridin-3-ylamine in 6 mL of 12M HCl at −20° C. were added a solution of 0.36 g (5.2 mmol, 1.3 eq) of sodium nitrite dissolved in 2 mL of H20. The reaction mixture was stirred for 15 min, and 4.4 g (19.5 mmol, 5 eq) of tin chloride dihydrate dissolved in 2 mL of 12M HCl were added. The reaction mixture was allowed to reach 0° C. within 40 min, and the white precipitate was recovered by filtration and washed with Et2O to yield 0.35 g (62%) of (6-chloro-pyridin-3-yl)-hydrazine hydrochloride as a white solid, MS: 144 (MH+).

후처리

  1. dissolutiondissolved in 2 mL of H20
  2. additionwere added
  3. waitto reach 0° C. within 40 min
  4. filtrationthe white precipitate was recovered by filtration
  5. washwashed with Et2O

출처 및 근거

ORD 기록
ord-24fa16e79f334b7f8284040577a22e4b
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07906546B2

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