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Sodium Carbonate → HCID 70489858、化合物

HRID 462436
ノート
印刷プレビュー

反応式

HRID 462436 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 10340Sodium Carbonate2 回HCID 24489Sodium DithioniteHCID 12888901HCID 12888901、化合物HCID 713219382-{[1-(Aziridin-1-yl)-2-nitroethenyl]amino}ethan-1-ol

生成物 1

HCID 70489858HCID 70489858、化合物収率 69.7%

試薬・触媒・溶媒 3

HCID 887
Methanol
溶媒
HCID 962Water溶媒
HCID 3283Diethyl Ether溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-bff2372a294a4c99b982a52e8633f784
出典データセット
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04515806

反応ノート

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