Diethyl Ether → HCID 53777110、化合物

HRID 477302

反応式

HRID 477302 の反応式
[CH2:1]1[CH2:11][C:9](=[O:10])[C:8]2[C:3](=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:2]1.F[B-](F)(F)F.[CH3:17][N:18]([CH3:30])[C:19]([C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:20][CH:21]=[N+](C)C.CC[O-].[Na+].C(OCC)C>C(O)C>[CH:19]([O:10][CH:9]([CH3:8])[CH3:11])([CH3:25])[CH3:20].[CH3:17][N:18]([CH3:30])[C:19](=[CH:20][CH:21]=[C:11]1[CH2:1][CH2:2][C:3]2[C:8](=[CH:7][CH:6]=[CH:5][CH:4]=2)[C:9]1=[O:10])[C:25]([O:27][CH2:28][CH3:29])=[O:26]

参加物

7

反応物 4

HCID 3283Diethyl EtherHCID 107241-TetraloneHCID 2723922Sodium ethoxideHCID 86743575N-(dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate

生成物 2

HCID 7914Diisopropyl EtherHCID 53777110HCID 53777110、化合物収率 33.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
20 °C

実験手順

α-Tetralone (51 g) is added dropwise in the course of 45 minutes, at a temperature in the region of 15° C., to a mixture of N-(3-dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate (100 g) in ethanol (500 cc) and a 2M ethanolic solution of sodium ethylate (210 cc). The mixture is maintained for 1 hour 45 minutes at a temperature in the region of 20° C. and is then heated for 4 hours 45 minutes to 70° C. The reaction ethanol is evaporated off to dryness and the oil obtained is pounded with ethyl ether (4×300 cc). The ethereal extracts are concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa). After recrystallization of the solid obtained in a boiling mixture (60 cc) of isopropyl ether and ethyl acetate (90:10 by volume), ethyl 2-dimethylamino-4-(1-oxo-1,2,3,4-tetrahydro-2-naphthylidene)-2-butenoate (17.5 g), m.p. 84° C., is obtained.

後処理

  1. temperatureis then heated for 4 hours 45 minutes to 70° C
  2. customis evaporated off to dryness
  3. customthe oil obtained
  4. concentrationThe ethereal extracts are concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa)
  5. customAfter recrystallization of the solid

出典と根拠

ORDレコード
ord-9c589d637e044b4ea5c51eaf5dac36c2
出典データセット
uspto-grants-1989_12
特許番号
US04886835

関連ノート

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