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

HRID 1758459

反応式

HRID 1758459 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3df3fb0889284f939f538ddcc18be3a7
出典データセット
uspto-grants-1983_02
特許番号
US04374040

関連ノート

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