Hydrochloric Acid → 2-Hydroxy-5,5-dimethyl-4-(2-naphthyl)-1,3,2-dioxaphosphorinane 2-oxide

HRID 1815671

반응식

HRID 1815671 반응식
[OH-:1].[Na+].Cl[P:4]1(=[O:22])[O:9][CH:8]([C:10]2[CH:19]=[CH:18][C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH:11]=2)[C:7]([CH3:21])([CH3:20])[CH2:6][O:5]1.Cl>O>[OH:1][P:4]1(=[O:22])[O:9][CH:8]([C:10]2[CH:19]=[CH:18][C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH:11]=2)[C:7]([CH3:21])([CH3:20])[CH2:6][O:5]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 22501140HCID 22501140, 화합물

생성물 1

HCID 225011422-Hydroxy-5,5-dimethyl-4-(2-naphthyl)-1,3,2-dioxaphosphorinane 2-oxide수율 93.2%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
101 °C

실험 절차

Sodium hydroxide (14.9 g, 0.373 mol) was dissolved in water (150 ml). To this solution was added little by little 2-chloro-5,5-dimethyl-4-(2-naphthyl)-1,3,2-dioxaphosphorinane-2-one (38.6 g, 0.124 mol) with heating to 100 to 102° C. and stirring for 30 min. The solution was stirred at the same temperature for 20 min, and the reaction solution was cooled to 45° C. Concentrated hydrochloric acid (37 ml) was added thereto to adjust the solution to acidic. The solution was stirred at 15° C. for 30 min. The crystals were collected by filtration, washed with water and then ether, and dried under reduced pressure at 60° C. to give the title compound as pale ocher crystals having the melting point of 237 to 238° C. (33.87 g, yield 93.2%).

후처리

  1. stirringThe solution was stirred at the same temperature for 20 min
  2. temperaturethe reaction solution was cooled to 45° C
  3. stirringThe solution was stirred at 15° C. for 30 min
  4. filtrationThe crystals were collected by filtration
  5. washwashed with water
  6. dry with materialether, and dried under reduced pressure at 60° C.

출처 및 근거

ORD 기록
ord-6728267f7ede4acbae692046d7b01c01
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06878831B2

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