Toluene → HCID 46831040, 화합물

HRID 446206노트

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HRID 446206 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 46831040HCID 46831040, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-5588399d70194e329514ba6a3af8e13e
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476470B2

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