Isopropylamine → HCID 178443204、化合物

HRID 359935ノート

反応式

HRID 359935 の反応式
[C:1](#[N:5])[CH2:2][C:3]#[N:4].Cl[CH2:7][C:8](Cl)=[O:9].[CH2:11]([NH2:24])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23].C(N)(C)C>CN(C=O)C.C(N(CC)CC)C>[NH2:4][C:3]1[N:24]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[CH2:7][C:8](=[O:9])[C:2]=1[C:1]#[N:5]

参加物

7

反応物 4

HCID 6363IsopropylamineHCID 6577Chloroacetyl chlorideHCID 8010MalononitrileHCID 40761Tridecanamine

生成物 1

HCID 178443204HCID 178443204、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒

反応条件

温度
0 °C

実験手順

19.8 g of malononitrile were dissolved in 30 ml of DMF and cooled to 0° C. While cooling, 61 g of triethylamine and 27 g of chloroacetyl chloride were simultaneously added dropwise to this, and the mixture was stirred at 10° C. for 10 minutes. 65.7 g of tridecylamine were then added dropwise, and the reaction mixture was stirred at room temperature for 48 hours. 300 ml of isopropylamine were then added to the mixture, which was refluxed for 2 hours, 10 g of active carbon were added, and the mixture was filtered hot. After cooling, the precipitate was filtered off with suction, washed and dried at 50° C. 40 g (44% of theory) of the compound of the formula ##STR25## of melting point 214° to 215° C. were obtained. The IR, NMR, UV and mass spectra and the elemental analysis are consistent with the structural formula.

後処理

  1. temperatureWhile cooling
  2. stirringthe reaction mixture was stirred at room temperature for 48 hours
  3. temperaturewas refluxed for 2 hours
  4. addition10 g of active carbon were added
  5. filtrationthe mixture was filtered hot
  6. temperatureAfter cooling
  7. filtrationthe precipitate was filtered off with suction
  8. washwashed
  9. customdried at 50° C
  10. custom40 g (44% of theory) of the compound of the formula ##STR25## of melting point 214° to 215° C. were obtained

出典と根拠

ORDレコード
ord-4d2a89e19e394fb7bae643ae04a07e93
出典データセット
uspto-grants-1991_03
特許番号
US05003081

反応ノート

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