Water → 1'-(3,4-Dihydroquinolin-1(2h)-ylcarbonyl)spiro[indene-1,4'-piperidine]

HRID 551782ノート

反応式

HRID 551782 の反応式
[N:1]1([C:11]([O:13]C2C=CC([N+]([O-])=O)=CC=2)=O)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1.[CH2:23]1[C:28]2([C:36]3[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=3)[CH:30]=[CH:29]2)[CH2:27][CH2:26][NH:25][CH2:24]1.Cl.C(N(CC)CC)C.O>ClCCl>[N:1]1([C:11]([N:25]2[CH2:26][CH2:27][C:28]3([C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=[CH:29]3)[CH2:23][CH2:24]2)=[O:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 178488194-nitrophenyl 3,4-dihydroquinoline-1(2H)-carboxylateHCID 22509344Spiro[indene-1,4'-piperidine] hydrochloride

生成物 1

HCID 671900911'-(3,4-Dihydroquinolin-1(2h)-ylcarbonyl)spiro[indene-1,4'-piperidine]収率 85.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
150 °C

実験手順

0.4 g of 4-nitrophenyl 3,4-dihydroquinoline-1(2H)-carboxylate, 0.357 g of 4-spiroindene-piperidine hydrochloride, 0.28 ml of triethylamine and 2 ml of water are introduced into a 10 ml glass tube. The tube is sealed and then heated at 150° C. under microwave irradiation for 50 minutes. Dichloromethane is added. The organic phase is dried over magnesium sulfate and the solvent is evaporated under reduced pressure. The residue is chromatographed on silica gel with a heptane/ethyl acetate gradient from 9/1 to 0/1. 0.393 g of 1′-(3,4-dihydroquinolin-1(2H)-ylcarbonyl)spiro[indene-1,4′-piperidine] is obtained.

後処理

  1. customThe tube is sealed
  2. dry with materialThe organic phase is dried over magnesium sulfate
  3. customthe solvent is evaporated under reduced pressure
  4. customThe residue is chromatographed on silica gel with a heptane/ethyl acetate gradient from 9/1 to 0/1

出典と根拠

ORDレコード
ord-73587889789f4756bf820f8e03d376bf
出典データセット
uspto-grants-2011_05
特許番号
US07947834B2

反応ノート

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