Formaldehyde → Tetrahydro-N-methyl-N-(phosphonomethyl)-3-thiophenamine 1,1-dioxide

HRID 1758459

반응식

HRID 1758459 반응식
Cl.[CH3:2][NH:3][CH:4]1[CH2:8][CH2:7][S:6](=[O:10])(=[O:9])[CH2:5]1.[CH2:11]=O.[P:13]([OH:16])([OH:15])[OH:14].O>C(O)C>[CH3:2][N:3]([CH2:11][P:13]([OH:16])([OH:15])=[O:14])[CH:4]1[CH2:8][CH2:7][S:6](=[O:10])(=[O:9])[CH2:5]1

참가 물질

6

반응물 4

HCID 712FormaldehydeHCID 962WaterHCID 107909Phosphorous acidHCID 27708173-(Methylamino)-1lambda6-thiolane-1,1-dione hydrochloride

생성물 1

HCID 20509047Tetrahydro-N-methyl-N-(phosphonomethyl)-3-thiophenamine 1,1-dioxide수율 86.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of N-methyltetrahydro-3-thiophenamine 1,1-dioxide hydrochloride (37.2 parts, 0.20 mole); 90 percent paraformaldehyde (6.8 parts, 0.22 mole); orthophosphorous acid (18.0 parts, 0.22 mole); and water (30 parts) was heated at its reflux temperature for 3 hours. After cooling, the solution was stirred into ethanol (150 ml.) and the sticky, white precipitate was triturated under more ethanol. After being dried in vacuo over P2O5 the product weighed 42.0 g. (86.3 percent yield). m.p. 222°-225° C.

후처리

  1. temperaturereflux temperature for 3 hours
  2. temperatureAfter cooling
  3. customthe sticky, white precipitate was triturated under more ethanol
  4. dry with materialAfter being dried in vacuo over P2O5 the product

출처 및 근거

ORD 기록
ord-3df3fb0889284f939f538ddcc18be3a7
출처 데이터셋
uspto-grants-1983_02
특허 번호
US04374040

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