Hydrochloric Acid → 1H-Pyrrole, 2-(methylthio)-3-nitro-

HRID 1732607ノート

反応式

HRID 1732607 の反応式
Cl.[N+:2]([CH:5]=[C:6]([S:16][CH3:17])[NH:7][CH2:8][CH:9](OCC)OCC)([O-:4])=[O:3].C(=O)([O-])[O-].[K+].[K+]>CCOCC>[CH3:17][S:16][C:6]1[NH:7][CH:8]=[CH:9][C:5]=1[N+:2]([O-:4])=[O:3]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 71398340N-(2,2-Diethoxyethyl)-1-(methylsulfanyl)-2-nitroethen-1-amine

生成物 1

HCID 1516651H-Pyrrole, 2-(methylthio)-3-nitro-収率 54%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Dry hydrogen chloride was passed through a stirred solution of 1-nitro-2-methylthio-2-(2,2-diethoxyethylamino)-ethylene (9.7g, 0.04 mol) in dry ether (250 ml) at 5-10° for 3 hours. The resulting mixture was basified by pouring it into potassium carbonate solution (300 ml). The mixture was filtered to give a yellow solid, and the aqueous phase of the filtrate was separated and extracted with ether (2×150 ml). The combined ether solutions were evaporated to a residue. This residue and the solid filtered off earlier were recrystallised from acetone-chloroform to give 2-methylthio-3-nitropyrrole (3.4g, 54%) m.p. 212-213°.

後処理

  1. filtrationThe mixture was filtered
  2. customto give a yellow solid
  3. customthe aqueous phase of the filtrate was separated
  4. extractionextracted with ether (2×150 ml)
  5. customThe combined ether solutions were evaporated to a residue
  6. filtrationThis residue and the solid filtered off
  7. customearlier were recrystallised from acetone-chloroform

出典と根拠

ORDレコード
ord-8820c653236443d48bc9e30207b8c348
出典データセット
uspto-grants-1980_12
特許番号
US04238494

反応ノート

読み込み中…