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m-Chloroperbenzoic acid → HCID 58504127、化合物

HRID 2407699
ノート
印刷プレビュー

反応式

HRID 2407699 の反応式
ClC1C=C(C=CC=1)C(OO)=O.[NH:12]([C:19]1[C:24]([C:25]([NH2:27])=[O:26])=[CH:23][N:22]=[C:21](SC)[N:20]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(N(C(C)C)CC)(C)C.[C:39]1([C:45]2[CH:49]=[C:48]([CH2:50][N:51]3[CH2:56][CH2:55][CH:54]([CH2:57][NH2:58])[CH2:53][CH2:52]3)[O:47][N:46]=2)[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1>ClCCl.C(OCC)(=O)C>[NH:12]([C:19]1[C:24]([C:25]([NH2:27])=[O:26])=[CH:23][N:22]=[C:21]([NH:58][CH2:57][CH:54]2[CH2:53][CH2:52][N:51]([CH2:50][C:48]3[O:47][N:46]=[C:45]([C:39]4[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=4)[CH:49]=3)[CH2:56][CH2:55]2)[N:20]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 70297m-Chloroperbenzoic acidHCID 81531DiisopropylethylamineHCID 2958214-Anilino-2-(methylthio)-5-pyrimidinecarboxamideHCID 58504252HCID 58504252、化合物

生成物 1

HCID 58504127HCID 58504127、化合物収率 27.5%

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

3-Chloroperoxybenzoic acid (195 mg) was added to a 0° C. suspension of the compound prepared in Example 93 (100 mg) in dichloromethane (4 mL). The reaction was stirred one hour at room temperature. Diisopropylethylamine (0.669 mL) and the compound prepared in Example 9 (198 mg) were added and the mixture was stirred at room temperature for 18 hours. The reaction was diluted with ethyl acetate and sequentially washed with a saturated sodium bicarbonate solution and brine. The organics were dried over magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (concentrated aqueous ammonia:methanol:ethyl acetate=0.1:0.9:25) to obtain the title compound (51 mg) having the following physical data.

後処理

  1. stirringthe mixture was stirred at room temperature for 18 hours
  2. washsequentially washed with a saturated sodium bicarbonate solution and brine
  3. dry with materialThe organics were dried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography on silica gel (concentrated aqueous ammonia:methanol:ethyl acetate=0.1:0.9:25)

出典と根拠

ORDレコード
ord-2b81f81d2e8242fe8832b0d95e813af3
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809538B2

反応ノート

読み込み中…

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