Quinuclidine → n-DODECANOYLOXYMETHYLQUINUCLIDINIUM CHLORIDE

HRID 971474

反応式

HRID 971474 の反応式
[C:1]([O:14][CH2:15][Cl:16])(=[O:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[N:17]12[CH2:24][CH2:23][CH:20]([CH2:21][CH2:22]1)[CH2:19][CH2:18]2.[K+].[Br-]>CCOCC>[Cl-:16].[C:1]([O:14][CH2:15][N+:17]12[CH2:24][CH2:23][CH:20]([CH2:21][CH2:22]1)[CH2:19][CH2:18]2)(=[O:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

参加物

5

反応物 3

HCID 7527QuinuclidineHCID 253877Potassium BromideHCID 543634Chloromethyl dodecanoate

生成物 1

HCID 14128213n-DODECANOYLOXYMETHYLQUINUCLIDINIUM CHLORIDE

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

2.49 g (0.01 mol) chloromethyl n-dodecanoate and 1.12 g (0.01 mol) quinuclidine were mixed and allowed to react together at room temperature for 48 hrs. Anhydrous ether was added to the mixture and the mixture was triturated in anhydrous ether overnite. The solid was isolated by filtration under a nitrogen atmosphere and thoroughly washed with anhydrous ether. After drying in vacuo over calcium sulfate at room temperature, 2.1 g (0.006 mol), 17 was obtained as a white solid, mp 170°-172°; ir (KBr) 2960, 2930, 1765, 1470, 1120, 1090, 860 and 830 cm-1 ; pmr (CDCl3) δ 5.8 (s, 2H), 3.9 (t, 6H), 2.5 (t, 2H), 2.2 (m, 7H), 1.3 (bs, 18H) and 0.9 (t, 3H) ppm.

後処理

  1. customto react together at room temperature for 48 hrs
  2. customthe mixture was triturated in anhydrous ether overnite
  3. customThe solid was isolated by filtration under a nitrogen atmosphere
  4. washthoroughly washed with anhydrous ether
  5. dry with materialAfter drying in vacuo over calcium sulfate at room temperature
  6. custom2.1 g (0.006 mol), 17 was obtained as a white solid, mp 170°-172°

出典と根拠

ORDレコード
ord-856f122a45cb47ceb9e0c06037a5e544
出典データセット
uspto-grants-1979_07
特許番号
US04160099

関連ノート

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