Water → 2-(1,2,5-Thiadiazol-4-yl)-ethane-1,1-diphosphonic acid

HRID 867859

反応式

HRID 867859 の反応式
[S:1]1[N:5]=[C:4]([CH2:6][CH:7]([P:16]([O:21]CC)(=[O:20])[O:17]CC)[P:8]([O:13]CC)(=[O:12])[O:9]CC)[CH:3]=[N:2]1.C[Si](C)(C)Br.O>>[S:1]1[N:5]=[C:4]([CH2:6][CH:7]([P:16]([OH:21])(=[O:17])[OH:20])[P:8]([OH:13])(=[O:9])[OH:12])[CH:3]=[N:2]1

参加物

4

反応物 3

HCID 962WaterHCID 76113BromotrimethylsilaneHCID 21288947Tetraethyl 2-(1,2,5-thiadiazol-4-yl)-ethane-1,1-diphosphonate

生成物 1

HCID 212889202-(1,2,5-Thiadiazol-4-yl)-ethane-1,1-diphosphonic acid

実験手順

1.18 g. of the tetraethyl 2-(1,2,5-thiadiazol-4-yl)-ethane-1,1-diphosphonate described in Example 3 is mixed with 3.3 ml. trimethylbromosilane under an atmosphere of nitrogen. The reaction mixture is left to stand for 24 hours at ambient temperature and the solution is then evaporated, the residue is mixed with water, the solution is adjusted to a pH of 5 with sodium hydroxide and mixed with methanol. The precipitate obtained is filtered off with suction. There is thus obtained 0.56 g. (53% of theory)of the desired diphosphonic acid in the form of the disodium salt with 1 mole of water of crystallisation; m.p.>300° C.; Mrel =0.9.

後処理

  1. additionis mixed with 3.3 ml
  2. waitThe reaction mixture is left
  3. customthe solution is then evaporated
  4. additionthe residue is mixed with water
  5. additionmixed with methanol
  6. customThe precipitate obtained
  7. filtrationis filtered off with suction

出典と根拠

ORDレコード
ord-711d6f7d86f2493bab66a543b89d62b8
出典データセット
uspto-grants-1988_10
特許番号
US04777163

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