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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
ノート
印刷プレビュー

反応式

HRID 471052 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-561b327dd96a4689adf60e0ef719b103
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629271B2

反応ノート

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