Dimethylamine → (Dihydro-3,3-diphenyl-3H-furan-2-ylidene)dimethylammonium bromide

HRID 448810

反応式

HRID 448810 の反応式
[CH3:1][NH:2][CH3:3].C([O-])([O-])=O.[Na+].[Na+].[Br:10][CH2:11][CH2:12][C:13]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:14](Cl)=[O:15]>C1(C)C=CC=CC=1>[Br-:10].[CH3:1][N+:2]([CH3:3])=[C:14]1[C:13]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:12][CH2:11][O:15]1

参加物

5

反応物 3

HCID 674DimethylamineHCID 10340Sodium CarbonateHCID 222500664-Bromo-2,2-diphenylbutyric chloride

生成物 1

HCID 2723589(Dihydro-3,3-diphenyl-3H-furan-2-ylidene)dimethylammonium bromide収率 53%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of dimethylamine (2M in THF, 50 mL) and saturated aqueous Na2CO3 (100 mL) was added dropwise a solution of compound (E) in toluene (100 mL), prepared as described above, at 0° C. The resulting mixture was allowed to stir for 12 hours. The mixture was extracted with toluene (1×30 mL) and chloroform (3×100 mL). The combined extracts were washed with water (1×30 mL), dried over K2CO3. After evaporation to dryness and crystallization with methyl isobutyl ketone, the desired product (F) dimethyl(tetrahydro-3,3-diphenyl-2-furylidene)ammonium bromide was obtained in 53% yield.

後処理

  1. customprepared
  2. customat 0° C
  3. extractionThe mixture was extracted with toluene (1×30 mL) and chloroform (3×100 mL)
  4. washThe combined extracts were washed with water (1×30 mL)
  5. dry with materialdried over K2CO3
  6. customAfter evaporation
  7. customto dryness and crystallization with methyl isobutyl ketone

出典と根拠

ORDレコード
ord-5702575d28d6435ab8ea4995a21ad689
出典データセット
uspto-grants-2013_07
特許番号
US08481743B2

関連ノート

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