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o-Anisamide, 3-methyl- → HCID 21504428、化合物

HRID 1288272
ノート
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反応式

HRID 1288272 の反応式
[B-](F)(F)(F)F.[CH3:6][CH2:7][O+](CC)CC.[CH3:13][O:14][C:15]1[C:23]([CH3:24])=[CH:22][CH:21]=[CH:20][C:16]=1[C:17]([NH2:19])=[O:18]>C(Cl)Cl>[CH3:13][O:14][C:15]1[C:23]([CH3:24])=[CH:22][CH:21]=[CH:20][C:16]=1[C:17](=[NH:19])[O:18][CH2:6][CH3:7]
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 56081o-Anisamide, 3-methyl-HCID 2723982Triethyloxonium tetrafluoroborate

生成物 1

HCID 21504428HCID 21504428、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of triethyloxonium borofluoride (23 g.) in anhydrous methylene chloride (60 ml.) was added to a solution of 2-methoxy-3-methylbenzamide [19.7 g; prepared as described in French Patent M.21] in anhydrous methylene chloride (200 ml.). The mixture was kept at room temperature for 3 days, concentrated to about 120 ml. and diluted with anhydrous diethyl ether (300 ml.). The solid which separated was filtered off and washed with anhydrous diethyl ether to give ethyl 2-methoxy-3-methylbenzimidate borofluoride (28.7 g.), m.p. 93°-96° C., which was pure enough for use in the next stage of the synthesis. An aliquot was recrystallised from a mixture of anhydrous methylene chloride and anhydrous diethyl ether to give pure ethyl 2-methoxy-3-methylbenzimidate borofluoride, m.p. 102°-104° C.

後処理

  1. concentrationconcentrated to about 120 ml
  2. additionand diluted with anhydrous diethyl ether (300 ml.)
  3. customThe solid which separated
  4. filtrationwas filtered off
  5. washwashed with anhydrous diethyl ether

出典と根拠

ORDレコード
ord-cb29314ad3c640bda496207d73672de7
出典データセット
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03987160

反応ノート

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