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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
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HRID 1973675 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-52175175aa0b41a587499117a18b032b
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03998835

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