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

HRID 481821
ノート
印刷プレビュー

反応式

HRID 481821 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

HCID 19067334HCID 19067334、化合物収率 97.4%

試薬・触媒・溶媒 2

HCID 7237O-Xylene溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6fa06fa064dd409c8550f6759ba1bb36
出典データセット
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05789623

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート