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Dimethylamine → HCID 19819744、化合物

HRID 1031179
ノート
印刷プレビュー

反応式

HRID 1031179 の反応式
[CH3:1][NH:2][CH3:3].Cl[CH2:5][CH2:6][CH:7]1[N:20]([CH3:21])[C:12]2=[N:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[N:11]2[C:10](=[O:22])[N:9]([CH3:23])[CH2:8]1>CO>[OH2:22].[CH3:1][N:2]([CH3:3])[CH2:5][CH2:6][CH:7]1[N:20]([CH3:21])[C:12]2=[N:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[N:11]2[C:10](=[O:22])[N:9]([CH3:23])[CH2:8]1
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 674Dimethylamine2 回HCID 198197592-(2-Chloroethyl)-3,4-dihydro-1,4-dimethyl-1H-[1,3,5]triazepino[3,2-a]benzimidazol-5(2H)-one

生成物 1

HCID 19819744HCID 19819744、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 90 mL of freshly collected dimethylamine and 10 mL of methanol was added 3.25 g (0.011 mol) of 2-(2-chloroethyl)-3,4-dihydro-1,4-dimethyl-1H-[1,3,5]triazepino[3,2-a]benzimidazol-5(2H)-one. The reaction flask was sealed and left standing at room temperature for 6 days. The dimethylamine was then allowed to evaporate at room temperature and the residue partitioned between 75 mL of 1N NaOH and 75 mL of CH2Cl2. The organic phase was washed with another 50 mL of 1N NaOH. The combined organic layers were dried over Na2SO4, filtered, and concentrated by rotary evaporation. The solid residue was recrystallized from isopropyl ether to give 2.8 g of white analytically pure crystals, mp 91°-95° C.

後処理

  1. customThe reaction flask was sealed
  2. waitleft
  3. customto evaporate at room temperature
  4. customthe residue partitioned between 75 mL of 1N NaOH and 75 mL of CH2Cl2
  5. washThe organic phase was washed with another 50 mL of 1N NaOH
  6. dry with materialThe combined organic layers were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated by rotary evaporation
  9. customThe solid residue was recrystallized from isopropyl ether
  10. customto give 2.8 g of white analytically pure crystals, mp 91°-95° C.

出典と根拠

ORDレコード
ord-faa5d8b0e54c4a86a33383a9ef172c15
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05109013

反応ノート

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