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

HRID 1581916

반응식

HRID 1581916 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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.)

출처 및 근거

ORD 기록
ord-875c204cc1be47828cd8cebd74113a17
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06734158B2

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