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Triethylamine → HCID 86602052、化合物

HRID 1295367
ノート
印刷プレビュー

反応式

HRID 1295367 の反応式
C(N(CC)CC)C.[F:8][C:9]([F:25])([F:24])[C:10]1[CH:11]=[C:12]([C@@H:20]([NH:22][CH3:23])[CH3:21])[CH:13]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:15]=1.Cl[C:27](Cl)([O:29][C:30](=[O:36])OC(Cl)(Cl)Cl)Cl.[C:38]1([CH:44]2[NH:49][CH2:48][CH:47]3C2(CO)[CH2:46]3)[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1.C(N(C(C)C)CC)(C)C>C(Cl)Cl.C(#N)C>[C:38]1([C@@H:44]2[NH:49][CH2:48][CH:47]3[C@:27]2([O:29][C:30](=[O:36])[N:22]([C@H:20]([C:12]2[CH:11]=[C:10]([C:9]([F:24])([F:25])[F:8])[CH:15]=[C:14]([C:16]([F:17])([F:18])[F:19])[CH:13]=2)[CH3:21])[CH3:23])[CH2:46]3)[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=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

8

反応物 5

HCID 8471TriethylamineHCID 81531DiisopropylethylamineHCID 94429TriphosgeneHCID 11608744(S)-N-Methyl-1-[3,5-bis(trifluoromethyl)phenyl]ethylamineHCID 58907340HCID 58907340、化合物

生成物 1

HCID 86602052HCID 86602052、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒
HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

To a round bottom flask was added methylene chloride (12 mL), triethylamine (0.55 mL, 3.9 mmol), and [(S)-1-(3,5-bis-trifluoromethyl-phenyl)-ethyl]-methyl-amine (0.35 g, 1.3 mmol). The mixture was cooled to 0° C. and triphosgene (0.15 g, 0.50 mmol) in methylene chloride (4 mL) was added dropwise. The clear solution was stirred for 16 hours at room temperature. To the reaction mixture was added (2-phenyl-3-aza-bicyclo[3.1.0]hex-1-yl)-methanol (0.25 g, 1.2 mmol), diisopropyl ethyl amine (0.41 mL, 2.4 mmol), and acetonitrile (10 mL). The reaction was heated to remove the methylene chloride and then refluxed for 1 hour. The solvent was removed at reduced pressure and the residue partitioned between 0.25N HCl and methylene chloride, the organic phase was washed with saturated sodium bicarbonate solution, brine, dried over sodium sulfate, filtered, and concentrated to a quantitative yield of oil. This material was flash chromatographed on silica using a gradient of 20 to 40% EtOAc/Hexanes and the first eluted (Rf=0.39 (50% EtOAc/hexanes) spot was rechromatographed using prep TLC eluting with 5% MeOH/CHCl3 to afford the title compound as a mixture of diasteomers (0.031 g, 5.5% yield) and as an oil.

後処理

  1. temperatureThe reaction was heated
  2. customto remove the methylene chloride
  3. temperaturerefluxed for 1 hour
  4. customThe solvent was removed at reduced pressure
  5. customthe residue partitioned between 0.25N HCl and methylene chloride
  6. washthe organic phase was washed with saturated sodium bicarbonate solution, brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-c8201f0f28eb4523b4848641551424f1
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07241798B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート