Cysteamine Hydrochloride → 7-Oxa-1-thia-4-azaspiro[4.4]nonane, 6-methyl-

HRID 1581916

反応式

HRID 1581916 の反応式
Cl.[NH2:2][CH2:3][CH2:4][SH:5].[CH3:6][CH:7]1[C:11](=O)[CH2:10][CH2:9][O:8]1.[OH-].[Na+]>O>[CH3:6][CH:7]1[O:8][CH2:9][CH2:10][C:11]21[S:5][CH2:4][CH2:3][NH:2]2

参加物

5

反応物 3

HCID 9082Cysteamine HydrochlorideHCID 14798Sodium HydroxideHCID 18522Dihydro-2-methyl-3(2H)-furanone

生成物 1

HCID 129802457-Oxa-1-thia-4-azaspiro[4.4]nonane, 6-methyl-収率 90%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 15.4 g of 2-aminoethanethiol-HCl (0.13 mole) dissolved into 50 ml of water were added slowly 20 g of 2-methyl-3-tetrahydrofuranone (0.2 mole) (solution pH=2.7). The pH was kept to neutrality by adding 10% aqueous NaOH. After 1 hour, extraction of the water solution with Et2O, drying of the organic phase with MgSO4 and distillation of the crude product (Bp 1.7 mbar, 93°-96° C.) gave 18 g of the desired product (yield=90%). The product was obtained as a mixture of two diastereoisomers (isomers a and b).

後処理

  1. extractionextraction of the water solution with Et2O
  2. dry with materialdrying of the organic phase with MgSO4 and distillation of the crude product (Bp 1.7 mbar, 93°-96° C.)

出典と根拠

ORDレコード
ord-875c204cc1be47828cd8cebd74113a17
出典データセット
uspto-grants-2004_05
特許番号
US06734158B2

関連ノート

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