Nitrogen → HCID 67366300, 화합물

HRID 42812노트

반응식

HRID 42812 반응식
N#N.[CH3:3][C:4]1([C:9]2[S:13][CH:12]=[C:11]([CH2:14][N:15]3[N:19]=[C:18]([N+:20]([O-])=O)[CH:17]=[N:16]3)[CH:10]=2)[O:8][CH2:7][CH2:6][O:5]1.[NH4+].[Cl-]>CCO.O.[Fe]>[CH3:3][C:4]1([C:9]2[S:13][CH:12]=[C:11]([CH2:14][N:15]3[N:19]=[C:18]([NH2:20])[CH:17]=[N:16]3)[CH:10]=2)[O:8][CH2:7][CH2:6][O:5]1

참가 물질

7

반응물 3

HCID 947NitrogenHCID 25517Ammonium ChlorideHCID 673668552-[5-(2-Methyl-[1,3]dioxolan-2-yl)-thiophen-3-ylmethyl]-4-nitro-2H-[1,2,3]triazole

생성물 1

HCID 67366300HCID 67366300, 화합물

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
85 °C

실험 절차

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a mixture of 2-[5-(2-methyl-[1,3]dioxolan-2-yl)-thiophen-3-ylmethyl]-4-nitro-2H-[1,2,3]triazole (50 mg, 0.17 mmol), iron powder (29 mg, 0.51 mmol) and NH4Cl (46 mg, 0.84 mmol) in a mixture of EtOH (1.0 mL) and water (0.5 mL) was stirred at 85° C. for 15 min. The reaction mixture was filtered while hot and concentrated under reduced pressure. CH2Cl2 (10 mL) was added followed by 1N NaOH (10 mL). The aq. layer was extracted with CH2Cl2 (2×10 mL) and the combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a light yellow oil. LC-MS-conditions 02: tR=0.78 min; [M+H]+=267.28.

후처리

  1. filtrationThe reaction mixture was filtered while hot and
  2. concentrationconcentrated under reduced pressure
  3. additionCH2Cl2 (10 mL) was added
  4. extractionThe aq. layer was extracted with CH2Cl2 (2×10 mL)
  5. dry with materialextracts were dried over MgSO4
  6. filtrationfiltered
  7. customthe solvents were removed under reduced pressure

출처 및 근거

ORD 기록
ord-11ca429d47ed46f6a11e92bf49075ad3
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536209B2

반응 노트

불러오는 중…