Acetal → 1,3,5-Triazine-2,4-diamine, 3,6-dihydro-N2,N2,6-trimethyl-, hydrochloride (1:1)

HRID 575519

反応式

HRID 575519 の反応式
[CH3:1][N:2]([C:4]([N:6]=[C:7]([NH2:9])[NH2:8])=[NH:5])[CH3:3].[ClH:10].[CH2:11](OC(OCC)C)[CH3:12]>C(O)C(C)C.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[ClH:10].[NH2:8][C:7]1[NH:6][C:4]([N:2]([CH3:3])[CH3:1])=[N:5][CH:11]([CH3:12])[N:9]=1

参加物

5

反応物 2

HCID 7765AcetalHCID 14219Metformin Hydrochloride

生成物 1

HCID 101764861,3,5-Triazine-2,4-diamine, 3,6-dihydro-N2,N2,6-trimethyl-, hydrochloride (1:1)収率 77.6%

試薬・触媒・溶媒 2

HCID 521998p-Toluenesulfonic acid monohydrate触媒HCID 6560Isobutanol溶媒

反応条件

温度
10 °C

実験手順

Comparative experiment: A mixture of 250.2 g of metformin hydrochloride, 213.6 g of acetaldehyde diethyl acetal and 12.5 g of toluene-4-sulfonic acid monohydrate in 500 ml of isobutanol was heated under reflux for 40 hours. Some of the solvent was removed by distillation. The mixture was cooled to 10° C., and the white precipitate was separated off, giving 224.7 g (77.4%) of 4-amino-3,6-dihydro-2-dimethylamino-6-methyl-1,3,5-triazine hydrochloride.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 40 hours
  3. customSome of the solvent was removed by distillation
  4. customthe white precipitate was separated off

出典と根拠

ORDレコード
ord-353a30ee0b2a4526a7dcda44cf438138
出典データセット
uspto-grants-2015_05
特許番号
US09035048B2

関連ノート

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