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Triethylamine → Dibenzyl-{(1S,2R)-2-benzyloxy-1-(3,5-difluorobenzyl)-2-[(3R,5S,6S)-6-(1-fluorocyclohexylmethoxy)-5-methylmorpholin-3-yl]-ethyl}-amine

HRID 20430
ノート
印刷プレビュー

反応式

HRID 20430 の反応式
ClC(Cl)(OC(=O)OC(Cl)(Cl)Cl)Cl.[CH2:13]([O:20][C@H:21]([C@@H:47]1[NH:52][C@@H:51]([CH3:53])[CH:50]([OH:54])[O:49][CH2:48]1)[C@@H:22]([N:32]([CH2:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)[CH2:33][C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[CH2:23][C:24]1[CH:29]=[C:28]([F:30])[CH:27]=[C:26]([F:31])[CH:25]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(N(CC)CC)C.[F:62][C:63]1([CH2:69]O)[CH2:68][CH2:67][CH2:66][CH2:65][CH2:64]1.FC(F)(F)S(O[Si](C)(C)C)(=O)=O.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH2:40]([N:32]([CH2:33][C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[C@@H:22]([CH2:23][C:24]1[CH:25]=[C:26]([F:31])[CH:27]=[C:28]([F:30])[CH:29]=1)[C@H:21]([O:20][CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[C@H:47]1[CH2:48][O:49][C@@H:50]([O:54][CH2:69][C:63]2([F:62])[CH2:68][CH2:67][CH2:66][CH2:65][CH2:64]2)[C@H:51]([CH3:53])[NH:52]1)[C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=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 6

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 65367Trimethylsilyl triflate2 回HCID 94429TriphosgeneHCID 18342450(1-Fluorocyclohexyl)methanolHCID 68564040(3S,5R)-5-[(1R,2S)-1-benzyloxy-2-dibenzylamino-3-(3,5-difluorophenyl)-propyl]-3-methylmorpholin-2-ol

生成物 1

HCID 68560341Dibenzyl-{(1S,2R)-2-benzyloxy-1-(3,5-difluorobenzyl)-2-[(3R,5S,6S)-6-(1-fluorocyclohexylmethoxy)-5-methylmorpholin-3-yl]-ethyl}-amine収率 31.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

Add triphosgene (246 mg, 0.79 mmol) at room temperature to a solution of (3S,5R)-5-[(1R,2S)-1-benzyloxy-2-dibenzylamino-3-(3,5-difluorophenyl)-propyl]-3-methylmorpholin-2-ol (1 g, 1.75 mmol) and triethylamine (0.99 mL, 7 mmol) in anhydrous dichloromethane (17 mL). Stir for 30 min, cool to 0° C. and add (1-fluorocyclohexyl)-methanol (1.16 g, 8.75 mmol) and trimethylsilyl trifluoromethanesulfonate (TMSOTf) (0.64 mL, 3.5 mmol). Stir at 0° C. for 1 hour and at room temperature for 2 hours. Add more trimethylsilyl trifluoromethanesulfonate (0.16 mL, 0.87 mmol) and stir at room temperature for 30 min. Add 10% aqueous potassium carbonate, separate the organic layer and extract the aqueous layer with dichloromethane. Combine the organic layers, dry (sodium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 0:100 to 20:80 hexanes:ethyl acetate), to give the title compound as a colorless oil (375 mg).

後処理

  1. stirringStir at 0° C. for 1 hour and at room temperature for 2 hours
  2. stirringstir at room temperature for 30 min
  3. customseparate the organic layer
  4. extractionextract the aqueous layer with dichloromethane
  5. dry with materialdry (sodium sulfate)
  6. filtrationfilter
  7. concentrationconcentrate
  8. custompurify
  9. wash(silica gel chromatography, eluting with 0:100 to 20:80 hexanes:ethyl acetate)

出典と根拠

ORDレコード
ord-ff70de919aa443f1927ba715ffc76ddf
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07745438B2

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