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Trifluoroacetic acid → Spiro[1H-indene-1,4'-piperidin]-3(2H)-one trifluoroacetamide

HRID 2229264
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HRID 2229264 반응식
Cl.[O:2]=[C:3]1[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[C:5]2([CH2:10][CH2:9][N:8](C(C(NC(=O)C(N)(C)C)CC3C4C(=CC=CC=4)NC=3)=O)[CH2:7][CH2:6]2)[CH2:4]1.[F:37][C:38]([F:43])([F:42])[C:39](O)=[O:40].C1(OC)C=CC=CC=1>ClCCl>[F:37][C:38]([F:43])([F:42])[C:39]([NH2:8])=[O:40].[NH:8]1[CH2:9][CH2:10][C:5]2([C:31]3[C:36](=[CH:35][CH:34]=[CH:33][CH:32]=3)[C:3](=[O:2])[CH2:4]2)[CH2:6][CH2:7]1
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참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 18467074n-[1(r,s)-[(2,3-Dihydro-3-oxospiro [1h-indene-1,4'-piperidin]1'-yl)-carbonyl]-2-(indol-3-yl)ethyl]-2-amino-2-methylpropanamide hydrochloride

생성물 1

HCID 18467060Spiro[1H-indene-1,4'-piperidin]-3(2H)-one trifluoroacetamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of the intermediate from Step A in a 1:1:0.5 mixture of trifluoroacetic acid, dichloromethane and anisole was stirred for 1 hour and then concentrated and azeotroped from toluene to give the title compound. 1H NMR (200 MHz, CDCl3): 7.81-7.70 (m, 1H),7.62-7.45 (m, 2H), 7.22-7.15 (m, 1H), 3.72-3.58 (m, 2H), 3.29-3.04 (m, 2H), 2.70 (s, 2H), 2.47 (dt, 2H), 1.85-1.75 (m, 2H).

후처리

  1. concentrationconcentrated
  2. customazeotroped from toluene

출처 및 근거

ORD 기록
ord-c20e34aa5fdc4ce5a310e9186590702d
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06420376B1

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