Oxalic Acid → N,N-Dimethyl-5-[[[2-[(1-methylthio-2-nitroethenyl)amino]ethyl]thio]methyl]-2-furanmethanamine oxalate

HRID 1277990

반응식

HRID 1277990 반응식
CS[CH:3]([S:8][CH3:9])[CH2:4][N+:5]([O-:7])=[O:6].[NH2:10][CH2:11][CH2:12][S:13][CH2:14][C:15]1[O:19][C:18]([CH2:20][N:21]([CH3:23])[CH3:22])=[CH:17][CH:16]=1.[C:24]([OH:29])(=[O:28])[C:25]([OH:27])=[O:26]>O1CCOCC1>[C:24]([OH:29])(=[O:28])[C:25]([OH:27])=[O:26].[CH3:22][N:21]([CH3:23])[CH2:20][C:18]1[O:19][C:15]([CH2:14][S:13][CH2:12][CH2:11][NH:10][C:3]([S:8][CH3:9])=[CH:4][N+:5]([O-:7])=[O:6])=[CH:16][CH:17]=1

참가 물질

5

반응물 3

HCID 971Oxalic AcidHCID 1622035-(((2-Aminoethyl)thio)methyl)-N,N-dimethyl-2-furanmethanamineHCID 123722641,1-Bis(methylsulfanyl)-2-nitroethane

생성물 1

HCID 70539027N,N-Dimethyl-5-[[[2-[(1-methylthio-2-nitroethenyl)amino]ethyl]thio]methyl]-2-furanmethanamine oxalate수율 99.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

A solution of 1,1-bis(methylthio)-2-nitroethane (19.8 g) and 5-[[(2-aminoethyl)thio]methyl]-N,N-dimethyl-2-furanmethanamine (6.42 g) in dry dioxan (120 ml) was heated at 80° C. for 6 hours. Oxalic acid (3.8 g) in dry dioxan (40 ml) was added and the crystalline solid which separated was filtered, washed with dioxan and dried to give the title compound (12.55 g) m.p. 140°-143° C.

후처리

  1. customthe crystalline solid which separated
  2. filtrationwas filtered
  3. washwashed with dioxan
  4. customdried

출처 및 근거

ORD 기록
ord-9f864dffe3924553b53db590a22afe22
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04279911

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