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Tetrabutylammonium Fluoride → 10-Bromo-6-(((tert-butyldimethylsilyl)oxy)methyl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine-2-carboxamide

HRID 575281
ノート
印刷プレビュー

反応式

HRID 575281 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH:10]([CH2:12][O:13][Si:14]([C:17]([CH3:20])([CH3:19])[CH3:18])([CH3:16])[CH3:15])[CH2:9][N:8]3[CH:21]=[CH:22][N:23]=[C:7]3[C:6]=2[CH:24]=1.ClC1C=CC2OCCC3N(C=C(C([O:42][CH3:43])=O)N=3)C=2N=1.CCCC[N+:48](CCCC)(CCCC)CCCC.[F-]>O1CCCC1.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH:10]([CH2:12][O:13][Si:14]([C:17]([CH3:20])([CH3:18])[CH3:19])([CH3:15])[CH3:16])[CH2:9][N:8]3[CH:21]=[C:22]([C:43]([NH2:48])=[O:42])[N:23]=[C:7]3[C:6]=2[CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 2724141Tetrabutylammonium FluorideHCID 86693202Methyl 2-chloro-6,7-dihydroimidazo[1,2-d]pyrido[3,2-b][1,4]oxazepine-9 carboxylateHCID 8669331010-Bromo-6-(((tert-butyldimethylsilyl)oxy)methyl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine

生成物 1

HCID 8669330910-Bromo-6-(((tert-butyldimethylsilyl)oxy)methyl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine-2-carboxamide

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

10-bromo-6-(((tert-butyldimethylsilyl)oxy)methyl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine-2-carboxamide was prepared from 10-bromo-6-(((tert-butyldimethylsilyl)oxy)methyl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine using the same procedures as outlined for the synthesis of methyl 2-chloro-6,7-dihydroimidazo[1,2-d]pyrido[3,2-b][1,4]oxazepine-9 carboxylate. TBAF (1.7 g, 6.50 mmol, 2.00 equiv) was added in several batches to a stirred solution of this intermediate (1.6 g, 3.54 mmol, 1.00 equiv) in tetrahydrofuran (7 mL) at room temperature. After 1 h the resulting solution was diluted with ethyl acetate, washed with water and brine, dried over anhydrous sodium sulfate and concentrated under vacuum.

後処理

  1. washwashed with water and brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-2b7948c53a7a4632b8d0546b3e65233b
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09034866B2

反応ノート

読み込み中…

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