Toluene → HCID 46831040、化合物

HRID 446206ノート

反応式

HRID 446206 の反応式
[CH2:1]([O:3][C:4]([C:6]12[CH2:13][CH2:12][C:9]([NH:14][CH2:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)([CH2:10][CH2:11]1)[CH2:8][CH:7]2[OH:22])=[O:5])[CH3:2].C1(C)C=CC=CC=1.C(N(CC)CC)C.[CH3:37][S:38](Cl)(=[O:40])=[O:39]>O1CCCC1>[CH2:1]([O:3][C:4]([C:6]12[CH2:13][CH2:12][C:9]([NH:14][CH2:15][C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=3)([CH2:10][CH2:11]1)[CH2:8][CH:7]2[O:22][S:38]([CH3:37])(=[O:40])=[O:39])=[O:5])[CH3:2]

参加物

6

反応物 4

HCID 1140TolueneHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 46831039Ethyl 2-hydroxy-4-[(phenylmethyl)amino]bicyclo[2.2.2]octane-1-carboxylate

生成物 1

HCID 46831040HCID 46831040、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 4-(benzylamino)-2-hydroxybicyclo[2.2.2]octane-1-carboxylic acid ethyl ester (6.0 g, 19.8 mmol), there were added toluene (42.0 g), tetrahydrofuran (10.8 g) and triethylamine (4.0 g, 39.6 mmol) and then the resulting mixture was stirred. Methanesulfonyl chloride (2.9 g, 24.9 mmol) was added dropwise to the mixture, followed by the stirring thereof for one hour and 30 minutes. After quenching the reaction mixture with water, the resulting mixture was subjected to extraction procedures and the organic phase was quantitatively analyzed (according to the LC technique). As a result, the yield of the desired product was found to be 100% (the internal standard substance used was m-xylene).

後処理

  1. customfor one hour
  2. custom30 minutes
  3. customAfter quenching the reaction mixture with water
  4. extractionthe resulting mixture was subjected to extraction procedures

出典と根拠

ORDレコード
ord-5588399d70194e329514ba6a3af8e13e
出典データセット
uspto-grants-2013_07
特許番号
US08476470B2

反応ノート

読み込み中…