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Toluene → (2,2-Difluoro-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(5-methylthiophen-2-yl)methanone trifluoroacetate

HRID 471052
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HRID 471052 반응식
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[F:8][C:9]1([F:35])[CH2:14][N:13]([C:15]([C:17]2[S:18][C:19]([CH3:22])=[CH:20][CH:21]=2)=[O:16])[CH2:12][C:11]2([CH2:27][CH2:26][N:25](C(OC(C)(C)C)=O)[CH2:24][CH2:23]2)[O:10]1.C1(C)C=CC=CC=1>ClCCl>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[F:35][C:9]1([F:8])[CH2:14][N:13]([C:15]([C:17]2[S:18][C:19]([CH3:22])=[CH:20][CH:21]=2)=[O:16])[CH2:12][C:11]2([CH2:23][CH2:24][NH:25][CH2:26][CH2:27]2)[O:10]1
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참가 물질

5

반응물 3

HCID 1140TolueneHCID 6422Trifluoroacetic acidHCID 57989071Tert-butyl 2,2-difluoro-4-(5-methylthiophene-2-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate

생성물 1

HCID 67291912(2,2-Difluoro-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(5-methylthiophen-2-yl)methanone trifluoroacetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (5 mL) was added to a solution of tert-butyl 2,2-difluoro-4-(5-methylthiophene-2-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate (example 37, step d) (0.4 g) in dichloromethane (20 mL) at 20° C. The solution was allowed to stand at 20° C. for 25 minutes. Toluene (40 mL) was added and the solvents were removed under reduced pressure. The residue was evaporated down twice with acetonitrile. The resultant gum was triturated with ether to afford the subtitled compound. Yield 0.39 g.

후처리

  1. customthe solvents were removed under reduced pressure
  2. customThe residue was evaporated down twice with acetonitrile
  3. customThe resultant gum was triturated with ether

출처 및 근거

ORD 기록
ord-561b327dd96a4689adf60e0ef719b103
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08629271B2

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