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Boron trifluoride etherate → HCID 67281057、化合物

HRID 1694725
ノート
印刷プレビュー

反応式

HRID 1694725 の反応式
B(F)(F)F.CCOCC.[F:10][C:11]([F:30])([F:29])[C:12]1[CH:28]=[CH:27][C:15]([O:16][CH2:17][C:18]([O:20][CH2:21][C:22]2([CH3:26])[CH2:25][O:24][CH2:23]2)=[O:19])=[CH:14][CH:13]=1>ClCCl>[CH3:23][C:22]12[CH2:25][O:24][C:18]([CH2:17][O:16][C:15]3[CH:27]=[CH:28][C:12]([C:11]([F:30])([F:29])[F:10])=[CH:13][CH:14]=3)([O:19][CH2:26]1)[O:20][CH2:21]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8000Boron trifluoride etherateHCID 86609219[4-(Trifluoromethyl)phenoxy]-acetic acid, (3-methyl-3-oxetanyl)methyl ester

生成物 1

HCID 67281057HCID 67281057、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Boron trifluoride diethyl etherate (1.48 ml) was added to a solution of the product from step (ii) (14.2 g) in dichloromethane at −78° C. The cooling bath was removed, the mixture, stirred for 3 h then triethylamine (6.2 ml) added. The mixture was reduced to half the volume under reduced pressure then filtered. The filtrate was evaporated under reduced pressure then the residue purified by chromatography on silica (pre-eluted with one column volume of neat triethylamine) eluting with dichloromethane, yield 11.1 g.

後処理

  1. customThe cooling bath was removed
  2. additiontriethylamine (6.2 ml) added
  3. filtrationthen filtered
  4. customThe filtrate was evaporated under reduced pressure
  5. customthe residue purified by chromatography on silica (pre-eluted with one column volume of neat triethylamine)
  6. washeluting with dichloromethane, yield 11.1 g

出典と根拠

ORDレコード
ord-8874e256ae6c4f94aecef261fbcafe04
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08158820B2

反応ノート

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