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6H-Dibenz[c,e][1,2]oxaphosphorin, 6-chloro- → HCID 19067334, 화합물

HRID 481821
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HRID 481821 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.[F:16][C:17]([F:31])([F:30])[C:18]1[CH:19]=[C:20]([Mg]Br)[CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:23]=1>CC1C=CC=CC=1C.O1CCCC1>[F:16][C:17]([F:31])([F:30])[C:18]1[CH:19]=[C:20]([P:2]([C:20]2[CH:21]=[C:22]([C:24]([F:27])([F:25])[F:26])[CH:23]=[C:18]([C:17]([F:16])([F:31])[F:30])[CH:19]=2)[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[OH:3])[CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:23]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 898166H-Dibenz[c,e][1,2]oxaphosphorin, 6-chloro-HCID 178506227HCID 178506227, 화합물

생성물 1

HCID 19067334HCID 19067334, 화합물수율 97.4%

시약·촉매·용매 2

HCID 7237O-Xylene용매HCID 8028Tetrahydrofuran용매

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온도
120 °C

실험 절차

23.5 g (0.1 mol) of 6-chloro-6H-dibenz[c,e][1,2]oxaphosphorine in 200 ml of anhydrous o-xylene at 80° C. are introduced, in an argon atmosphere with stirring, and a solution of 0.23 mol of 3,5-di(trifluoromethyl)phenylmagnesium bromide in 300 ml of tetrahydrofuran is added dropwise. Tetrahydrofuran is distilled off and the temperature is slowly increased to 120° C. in the course of this. The mixture is then stirred for 3 hours at 120° C., 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. 61.0 g of black solid are obtained. By recrystallization from heptane, with addition of activated carbon, and subsequent hot filtration, 37.2 g (59%) of pale yellow crystals having melting point 120° to 121° C. are obtained.

후처리

  1. distillationTetrahydrofuran is distilled off
  2. stirringThe mixture is then stirred for 3 hours at 120° C.
  3. temperaturecooled to room temperature
  4. addition100 ml of water are added
  5. customthe organic phase is separated off
  6. dry with materialdried with sodium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6fa06fa064dd409c8550f6759ba1bb36
출처 데이터셋
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05789623

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