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3-Tert-butylamino-1,2-propanediol → 1-Tert.butylamino-3-(2-methyl-4-thieno[3,2-c]pyridinyloxy)-2-propanol

HRID 1973675
ノート
印刷プレビュー

反応式

HRID 1973675 の反応式
[K].[C:2]([NH:6][CH2:7][CH:8]([OH:11])[CH2:9][OH:10])([CH3:5])([CH3:4])[CH3:3].Cl[C:13]1[C:18]2[CH:19]=[C:20]([CH3:22])[S:21][C:17]=2[CH:16]=[CH:15][N:14]=1>C(O)(C)(C)C>[C:2]([NH:6][CH2:7][CH:8]([OH:11])[CH2:9][O:10][C:13]1[C:18]2[CH:19]=[C:20]([CH3:22])[S:21][C:17]=2[CH:16]=[CH:15][N:14]=1)([CH3:5])([CH3:4])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 908313-Tert-butylamino-1,2-propanediolHCID 5462222PotassiumHCID 181763724-Chloro-2-methylthieno[3,2-c]pyridine

生成物 1

HCID 214903061-Tert.butylamino-3-(2-methyl-4-thieno[3,2-c]pyridinyloxy)-2-propanol

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

0.49 g of potassium are dissolved with heating in 60 cc of tert.butanol. After cooling, 1.5 g of 1-tert.butylamino-2,3-dihydroxypropane was added and subsequently 1.85 g of 4-chloro-2-methylthieno[3,2-c]pyridine was added. After stirring for one day at room temperature, heating is effected to 50° for a further day. The reaction solution is concentrated in a vacuum, the residue is taken up in 1 N hydrochloric acid and ether, the aqueous phase is neutralized with 2 N soda solution and extracted with methylene chloride. After drying over magnesium sulphate and concentrating, the title compound is obtained as an oil, which yields the hydrogen maleate having an M.P. of 210°-213°, with maleic acid in tetrahydrofuran.

後処理

  1. temperatureAfter cooling
  2. temperatureheating
  3. waitis effected to 50° for a further day
  4. concentrationThe reaction solution is concentrated in a vacuum
  5. extractionextracted with methylene chloride
  6. dry with materialAfter drying over magnesium sulphate
  7. concentrationconcentrating

出典と根拠

ORDレコード
ord-52175175aa0b41a587499117a18b032b
出典データセット
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03998835

反応ノート

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