4,5,6,7-Tetrahydro-N6-propyl-2,6-benzothiazolediamine → HCID 86591096、化合物

HRID 1835616

反応式

HRID 1835616 の反応式
[NH2:1][C:2]1[S:3][C:4]2[CH2:10][CH:9]([NH:11][CH2:12][CH2:13][CH3:14])[CH2:8][CH2:7][C:5]=2[N:6]=1.[C:15]([OH:24])(=[O:23])[C@@H:16]([C@H:18]([C:20]([OH:22])=[O:21])[OH:19])[OH:17]>CO>[CH3:14][CH2:13][CH2:12][NH:11][C@@H:9]1[CH2:10][C:4]2[S:3][C:2]([NH2:1])=[N:6][C:5]=2[CH2:7][CH2:8]1.[C:20]([CH:18]([CH:16]([C:15]([O-:24])=[O:23])[OH:17])[OH:19])([O-:22])=[O:21]

参加物

4

反応物 2

HCID 48854,5,6,7-Tetrahydro-N6-propyl-2,6-benzothiazolediamineHCID 444305L-Tartaric acid

生成物 1

HCID 86591096HCID 86591096、化合物収率 56.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

5 g of (±)2-amino-6-propylamino-4,5,6,7-tetrahydrobenzothiazole was dissolved in 25 ml of methanol and 4.0 g of L(+)-tartaric acid was added under stirring. The mixture was cooled and the white crystals were filtered off, washed with methanol and dried to yield 4.8 g of pramipexole tartrate. The crystals were dissolved in 10 ml of water and concentrated hydrochloric acid was added to dissolve the solid. The solution was cooled to 10° C. and a solution of 10 g of potassium hydroxide in 10 ml of water was added. The mixture was stirred for 30 minutes and the white crystals were removed by filtration and washed with cold water. The crystals were redissolved in 7 ml of ethanol and gaseous hydrogen chloride was bubbled through the solution at 10° C. After 1 hour of stirring, the precipitated solid was separated by filtration, washed with cold ethanol and dried to yield 2.1 g of white crystals. The product is identical with pramipexole dihydrochloride by NMR and has optical rotation [α](20,D)=−48,78° (c=1, MEOH)

後処理

  1. temperatureThe mixture was cooled
  2. filtrationthe white crystals were filtered off
  3. washwashed with methanol
  4. customdried

出典と根拠

ORDレコード
ord-d6b73e00d1b74e949e541fb38c58f090
出典データセット
uspto-grants-2004_08
特許番号
US06770761B2

関連ノート

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