Hydrochloric Acid → HCID 19067317, 화합물

HRID 481816

반응식

HRID 481816 반응식
Cl[P:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]2[CH:12]=[CH:13][CH:14]=[CH:15][C:4]=2[O:3]1.[C:16]1([Mg]Br)[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18][CH:17]=1.O.Cl>CC1C=CC=CC=1C.O1CCCC1>[OH:3][C:4]1[CH:15]=[CH:14][CH:13]=[CH:12][C:5]=1[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[P:2]([C:24]1[C:25]2[C:20](=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:21]=[CH:22][CH:23]=1)[C:16]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18][CH:17]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 898166H-Dibenz[c,e][1,2]oxaphosphorin, 6-chloro-HCID 178418298HCID 178418298, 화합물

생성물 1

HCID 19067317HCID 19067317, 화합물수율 69.7%

시약·촉매·용매 2

HCID 7237O-Xylene용매HCID 8028Tetrahydrofuran용매

실험 절차

14.1 g (60 mmol) of 6-chloro-6H-dibenz[c,e][1,2]-oxaphosphorine in 50 ml of anhydrous o-xylene are introduced, in an argon atmosphere with stirring, and a solution of 150 mmol of 1-naphthylmagnesium bromide in tetrahydrofuran is added dropwise. The temperature increases in the course of this from 25° to 45° C. The mixture is then stirred for 3 hours at 80° C. and 5 hours at 120° C. The mixture is cooled to room temperature and 100 ml of water are added. The mixture is neutralized with dilute hydrochloric acid, the organic phase is separated off, dried with sodium sulfate and concentrated under reduced pressure. 19.0 g of colorless oil are obtained. By crystallization with methanol/water, 10:1, 22.8 g (89%) of colorless crystals having melting point 255° to 256° C. are obtained.

후처리

  1. temperatureThe temperature increases in the course of this from 25° to 45° C
  2. stirringThe mixture is then stirred for 3 hours at 80° C. and 5 hours at 120° C
  3. customthe organic phase is separated off
  4. dry with materialdried with sodium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-01a57633005444b38d0d21b92fc20fa6
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05789623

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