Sodium Hydroxide → (3,4-Dihydro-2H-pyrido[3,2-b][1,4]thiazin-6-yl)methanol

HRID 1437328노트

반응식

HRID 1437328 반응식
O=[C:2]1[CH2:7][S:6][C:5]2[CH:8]=[CH:9][C:10]([C:12](OC)=[O:13])=[N:11][C:4]=2[NH:3]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1.CCOCC.C(Cl)(Cl)Cl>[S:6]1[CH2:7][CH2:2][NH:3][C:4]2[N:11]=[C:10]([CH2:12][OH:13])[CH:9]=[CH:8][C:5]1=2

참가 물질

8

반응물 4

HCID 14798Sodium HydroxideHCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydrideHCID 21873660Methyl 3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]thiazine-6-carboxylate

생성물 1

HCID 18454501(3,4-Dihydro-2H-pyrido[3,2-b][1,4]thiazin-6-yl)methanol수율 59.3%

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 6212Chloroform용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of methyl 3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]thiazine-6-carboxylate (1 g) (1.0 g) in dry tetrahydrofuran (170 ml) was treated with a 1M solution of lithium aluminium hydride in ether (14 ml) and the mixture was heated under reflux for 18 hours. It was cooled and a slight excess of 2N sodium hydroxide was added followed by chloroform and anhydrous sodium sulphate and the mixture was stirred for 30 minutes and filtered. The solution was evaporated to dryness to give a semi-solid (0.482 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 18 hours
  3. temperatureIt was cooled
  4. filtrationfiltered
  5. customThe solution was evaporated to dryness

출처 및 근거

ORD 기록
ord-e8a6a32f0468407a9dc62649dd0f1127
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07622481B2

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