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Triethylamine → 2-(4-Bromo-2,6-difluorophenyl)-2-(4-ethyl-3-oxo-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)acetamide

HRID 1525934
ノート
印刷プレビュー

反応式

HRID 1525934 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([CH:9](O)[C:10]([NH2:12])=[O:11])=[C:4]([F:14])[CH:3]=1.C(N(CC)CC)C.CS(Cl)(=O)=O.S([O-])(=O)(=O)C.Cl.[CH2:33]([N:35]1[CH2:40][C:39]2([CH2:45][CH2:44][NH:43][CH2:42][CH2:41]2)[O:38][CH2:37][C:36]1=[O:46])[CH3:34]>C(#N)C>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([CH:9]([N:43]2[CH2:44][CH2:45][C:39]3([O:38][CH2:37][C:36](=[O:46])[N:35]([CH2:33][CH3:34])[CH2:40]3)[CH2:41][CH2:42]2)[C:10]([NH2:12])=[O:11])=[C:4]([F:14])[CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8471Triethylamine2 回HCID 31297Methanesulfonyl chlorideHCID 85257MethanesulfonateHCID 712710764-Ethyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one hydrochlorideHCID 712710952-(4-Bromo-2,6-difluorophenyl)-2-hydroxyacetamide

生成物 1

HCID 71270829
2-(4-Bromo-2,6-difluorophenyl)-2-(4-ethyl-3-oxo-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)acetamide
収率 121.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
40 °C

実験手順

To a solution of 2-(4-bromo-2,6-difluorophenyl)-2-hydroxyacetamide (0.86 g, 3.2 mmol) and triethylamine (1.4 mL, 9.7 mmol) in anhydrous acetonitrile (5 mL) was added neat methanesulfonyl chloride (0.33 mL, 4.2 mmol). The reaction mixture was stirred vigorously at 40° C. for 3 h, at which point the reaction had progressed to completion. To this mesylate intermediate mixture was added more triethylamine (1.4 mL, 9.7 mmol) followed by 4-ethyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one hydrochloride (0.11 g, 0.48 mmol). The reaction mixture was heated at 90° C. for 3 h until the starting material was consumed. The reaction was diluted with water and was extracted with ether (3×35 mL). The combined ether phases were dried over sodium sulfate, filtered, and evaporated under reduced pressure. Purification of the residue by flash chromatography (65-100% of 10% methanol in dichloromethane:dichloromethane) afforded the title product (261 mg, 18% yield). MS(ES)+ m/e 446 [M+H]+; 1H NMR (400 MHz, CD2Cl2) δ ppm 1.12 (t, J=7.20 Hz, 3 H) 1.64-1.71 (m, 1 H) 1.73 (dd, J=4.17, 2.65 Hz, 1 H) 1.90-1.99 (m, 2 H) 2.19-2.27 (m, 1 H) 2.54-2.66 (m, 1 H) 2.67-2.73 (m, 1 H) 2.75-2.81 (m, 1 H) 3.15 (s, 2 H) 3.41 (q, J=6.91 Hz, 2 H) 3.98 (s, 2 H) 4.69 (s, 1 H) 5.68 (br. s., 1 H) 7.15-7.25 (m, 2 H) 7.36 (br. s., 1 H).

後処理

  1. temperatureThe reaction mixture was heated at 90° C. for 3 h until the starting material
  2. customwas consumed
  3. additionThe reaction was diluted with water
  4. extractionwas extracted with ether (3×35 mL)
  5. dry with materialThe combined ether phases were dried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customPurification of the residue by flash chromatography (65-100% of 10% methanol in dichloromethane:dichloromethane)

出典と根拠

ORDレコード
ord-0817fa3046784d9a99f99c62ea48fc7d
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09084794B2

反応ノート

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