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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Potassium Carbonate → Ranisen

HRID 1648822
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HRID 1648822 반응식
C(O)(=O)/C=C\C(O)=O.[CH3:9][N:10]([CH2:12][C:13]1[O:17][C:16]([CH2:18][S:19][C:20](=N)N)=[CH:15][CH:14]=1)[CH3:11].ClC[CH2:25][NH:26][C:27]([NH:32][CH3:33])=[CH:28][N+:29]([O-:31])=[O:30].C(=O)([O-])[O-].[K+].[K+]>O.O1CCCC1>[CH3:11][N:10]([CH2:12][C:13]1[O:17][C:16]([CH2:18][S:19][CH2:20][CH2:25][NH:26][C:27]([NH:32][CH3:33])=[CH:28][N+:29]([O-:31])=[O:30])=[CH:15][CH:14]=1)[CH3:9]
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참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 70486838HCID 70486838, 화합물HCID 71421354N~1~-(2-Chloroethyl)-N'~1~-methyl-2-nitroethene-1,1-diamine

생성물 1

HCID 5039Ranisen수율 19%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran
용매

실험 절차

A mixture of 1-[[[5-[(dimethylamino)methyl]-2-furanyl]-methyl]thio]methanimidamide maleate (1:2) (2.23 g), N-(2-chloroethyl)-N'-methyl-2-nitro-1,1-ethenediamine (0.9 g) and potassium carbonate (3.46 g) in water (10 ml) and tetrahydrofuran (10 ml) was stirred under nitrogen at room temperature for 5 days. The suspension was evaporated in vacuo; the residue suspended in water (50 ml) and extracted with ether (2×40 ml). The aqueous fraction was evaporated in vacuo and magnesium sulphate and tetrahhydrofuran (100 ml) added. After 18 hours, the mixture was filtered and the filtrate evaporated to give a semi-solid which was chromatographed (silica/methanol). The appropriate eluate was evaporated in vacuo to give the title compound (0.3 g), which had an n.m.r. identical to that of the product according to Example 1 above.

후처리

  1. customThe suspension was evaporated in vacuo
  2. extractionextracted with ether (2×40 ml)
  3. customThe aqueous fraction was evaporated in vacuo and magnesium sulphate and tetrahhydrofuran (100 ml)
  4. additionadded
  5. waitAfter 18 hours
  6. filtrationthe mixture was filtered
  7. customthe filtrate evaporated
  8. customto give a semi-solid which
  9. customwas chromatographed (silica/methanol)
  10. customThe appropriate eluate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-a45c1f3dc44849c4a1d96b059fb982f2
출처 데이터셋
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04413135

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