Acetone → HCID 13592264, 화합물

반응식

[OH:1][CH2:2][C:3]([CH2:12][OH:13])([CH2:8][N:9]=[N+:10]=[N-:11])[CH2:4][N:5]=[N+:6]=[N-:7].S(=O)(=O)(O)O.[OH-].[Ca+2].[OH-].[CH3:22][C:23]([CH3:25])=O>>[N:5]([CH2:4][C:3]1([CH2:8][N:9]=[N+:10]=[N-:11])[CH2:12][O:13][C:23]([CH3:25])([CH3:22])[O:1][CH2:2]1)=[N+:6]=[N-:7]

참가 물질

반응물 4

HCID 180Acetone

HCID 1118Sulfuric Acid

HCID 6093208Calcium Hydroxide

HCID 121709631,3-Propanediol, 2,2-bis(azidomethyl)-

생성물 1

HCID 13592264HCID 13592264, 화합물

실험 절차

1 mole of compound 1 was dissolved in 500 ml of dry acetone. After addition of 10 ml of concentrated sulfuric acid, the reaction mixture was stirred at room temperature for 2 hours. It was neutralized with calcium hydroxide and filtered and the filtrate and was concentrated to a syrup in vacuo. The crude product was further purified by column chromatography (eluting agent: chloroform/ethyl acetate 9:1).

후처리

filtrationfiltered
concentrationthe filtrate and was concentrated to a syrup in vacuo
customThe crude product was further purified by column chromatography (eluting agent: chloroform/ethyl acetate 9:1)

출처 및 근거

ORD 기록: ord-38408e9fe9c341309b31f5c87b7d13c1
출처 데이터셋: uspto-grants-1988_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04730069

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