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Sodium Carbonate → HCID 70489858, 화합물

HRID 462436
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HRID 462436 반응식
C(=O)([O-])[O-].[Na+].[Na+].C(O)(=O)C(O)=O.[CH3:13][N:14]([CH2:16][C:17]1[O:21][C:20]([CH2:22][SH:23])=[CH:19][CH:18]=1)[CH3:15].S(S([O-])=O)([O-])=O.[Na+].[Na+].[OH:32][CH2:33][CH2:34][NH:35][C:36](=[CH:40][N+:41]([O-:43])=[O:42])[N:37]1[CH2:39][CH2:38]1>O.CO.C(OCC)C>[CH3:15][N:14]([CH2:16][C:17]1[O:21][C:20]([CH2:22][S:23][CH2:39][CH2:38][NH:37][C:36]([NH:35][CH2:34][CH2:33][OH:32])=[CH:40][N+:41]([O-:43])=[O:42])=[CH:19][CH:18]=1)[CH3:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 10340Sodium Carbonate2회HCID 24489Sodium DithioniteHCID 12888901HCID 12888901, 화합물HCID 713219382-{[1-(Aziridin-1-yl)-2-nitroethenyl]amino}ethan-1-ol

생성물 1

HCID 70489858HCID 70489858, 화합물수율 69.7%

시약·촉매·용매 3

HCID 887
Methanol
용매
HCID 962Water용매
HCID 3283Diethyl Ether용매

실험 절차

Ethyl ether (15 ml) and an excess of anhydrous sodium carbonate were added to a mixture in water of 0.13 g (0.5 mmole) of 5-[(dimethylamino)methyl]-2-furanmethanethiol oxalate (1:1), sodium dithionite (0.05 g) and anhydrous sodium carbonate (0.15 g). The mixture was filtered and the filtrate was evaporated under vacuum. 0.087 g (0.5 mmole) of N-(2-hydroxyethyl)-alpha-(nitromethylene)-1-aziridinemethaneamine and 4 ml of methanol were added to the residue. The mixture was evaporated to dryness and the residue was heated to 95°-100° C. for 1 hour and chromatographed over silica (methanol-0.88 NH3 ; 79:1). The appropriate eluate was evaporated under vacuum to give 0.12 g of N-[2-[[(5-[(dimethylamino)methyl]-2-furanyl)methyl]thio]ethyl]-N'-(2-hydroxyethyl)-2-nitro-1,1-ethenediamine having the same properties as the product prepared according to Example 1, paragraph (a).

후처리

  1. filtrationThe mixture was filtered
  2. customthe filtrate was evaporated under vacuum
  3. customThe mixture was evaporated to dryness
  4. temperaturethe residue was heated to 95°-100° C. for 1 hour
  5. customchromatographed over silica (methanol-0.88 NH3 ; 79:1)
  6. customThe appropriate eluate was evaporated under vacuum

출처 및 근거

ORD 기록
ord-bff2372a294a4c99b982a52e8633f784
출처 데이터셋
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04515806

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