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Hydrochloric Acid → HCID 67111778、化合物

HRID 1177619
ノート
印刷プレビュー

反応式

HRID 1177619 の反応式
C(N(CC)CC)C.Cl.[NH2:9][CH:10]([CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]2[S:23][C:24]3[C:29]([N:30]=2)=[CH:28][CH:27]=[C:26]([C:31]2([C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)[CH2:33][CH2:32]2)[N:25]=3)=[C:18]([F:40])[CH:17]=1)[C:11]([OH:13])=[O:12].[CH3:41][C:42]([O:45][C:46](O[C:49]([O:51][C:52]([CH3:55])([CH3:54])[CH3:53])=[O:50])=[O:47])([CH3:44])[CH3:43].Cl>C1COCC1.O.CCOC(C)=O>[C:42]([O:45][C:46]([NH:9][C@H:10]([CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]2[S:23][C:24]3[C:29]([N:30]=2)=[CH:28][CH:27]=[C:26]([C:31]2([C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)[CH2:33][CH2:32]2)[N:25]=3)=[C:18]([F:40])[CH:17]=1)[C:11]([OH:13])=[O:12])=[O:47])([CH3:44])([CH3:43])[CH3:41].[C:52]([O:51][C:49]([NH:9][C@@H:10]([CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]2[S:23][C:24]3[C:29]([N:30]=2)=[CH:28][CH:27]=[C:26]([C:31]2([C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)[CH2:33][CH2:32]2)[N:25]=3)=[C:18]([F:40])[CH:17]=1)[C:11]([OH:13])=[O:12])=[O:50])([CH3:53])([CH3:54])[CH3:55]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 90495Di-tert-butyl dicarbonateHCID 67111648HCID 67111648、化合物

生成物 2

HCID 67111778HCID 67111778、化合物HCID 68635898HCID 68635898、化合物

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
2 回
HCID 8028Tetrahydrofuran溶媒2 回
HCID 8857Ethyl Acetate溶媒

実験手順

Triethylamine (0.0967 mL, 0.695 mmol) was added to a slurry of (rac)-2-amino-4-(3-fluoro-4-(5-(1-phenylcyclopropyl)thiazolo[5,4-b]pyridin-2-yl)phenyl)butanoic acid hydrochloride (0.153 g, 0.316 mmol) in THF (5.00 mL, 61.7 mmol) and WATER (5.00 mL, 278 mmol). The reaction mixture was cooled in an ice bath, and a solution of Boc2O (0.117 g, 0.537 mmol) in THF 2 mL was added dropwise, and the solution was then stirred at ambient temperature for 18 h. The reaction mixture was diluted with water and EtOAc, pH was adjusted to 5 with 1 N aq. HCl, and the aqueous layer was extracted with EtOAc. The combined organics were dried over MgSO4, filtered, and concentrated in vacuo, and the residue purified by chiral SFC (Column: Chiralpak AS-H (21×250 mm, 5 um); A: Liquid CO2; B: Methanol; Isocratic: 70:30 (A:B); Flow Rate: 70 mL/min) to give separately (R)-2-(tert-butoxycarbonylamino)-4-(3-fluoro-4-(5-(1-phenylcyclopropyl)-thiazolo[5,4-b]pyridin-2-yl)phenyl)butanoic acid and (S)-2-(tert-butoxycarbonylamino)-4-(3-fluoro-4-(5-(1-phenylcyclopropyl)thiazolo[5,4-b]pyridin-2-yl)phenyl)butanoic acid. MS (ESI) m/z: calculated: 547.2; Observed: 548.1 (M++1).

後処理

  1. temperatureThe reaction mixture was cooled in an ice bath
  2. extractionthe aqueous layer was extracted with EtOAc
  3. dry with materialThe combined organics were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customthe residue purified by chiral SFC (Column

出典と根拠

ORDレコード
ord-887664785de04783b4ffa3db720adffe
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07842685B2

反応ノート

読み込み中…

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