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

HRID 1437328

反応式

HRID 1437328 の反応式
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

参加物

8

反応物 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

生成物 1

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

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 6212Chloroform溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-e8a6a32f0468407a9dc62649dd0f1127
出典データセット
uspto-grants-2009_11
特許番号
US07622481B2

関連ノート

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