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Triethylamine → Gsk-2838232

HRID 513889
ノート
印刷プレビュー

反応式

HRID 513889 の反応式
Cl.[CH3:2][N:3]([CH3:7])[CH2:4][CH:5]=O.[Cl:8][C:9]1[CH:59]=[CH:58][C:12]([CH2:13][NH:14][CH2:15][C@@H:16]([C@:18]23[CH2:53][C:52](=[O:54])[C:51]([CH:55]([CH3:57])[CH3:56])=[C:19]2[C@@H:20]2[C@@:33]([CH3:36])([CH2:34][CH2:35]3)[C@@:32]3([CH3:37])[C@@H:23]([C@:24]4([CH3:50])[C@@H:29]([CH2:30][CH2:31]3)[C:28]([CH3:39])([CH3:38])[C@@H:27]([O:40][C:41](=[O:49])[CH2:42][C:43]([CH3:48])([CH3:47])[C:44]([OH:46])=[O:45])[CH2:26][CH2:25]4)[CH2:22][CH2:21]2)[OH:17])=[CH:11][CH:10]=1.CCN(CC)CC.C([BH3-])#N.[Na+]>CO.C(Cl)Cl.CCOC(C)=O.O>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:13][N:14]([CH2:5][CH2:4][N:3]([CH3:7])[CH3:2])[CH2:15][C@@H:16]([C@:18]23[CH2:53][C:52](=[O:54])[C:51]([CH:55]([CH3:56])[CH3:57])=[C:19]2[C@@H:20]2[C@@:33]([CH3:36])([CH2:34][CH2:35]3)[C@@:32]3([CH3:37])[C@@H:23]([C@:24]4([CH3:50])[C@@H:29]([CH2:30][CH2:31]3)[C:28]([CH3:38])([CH3:39])[C@@H:27]([O:40][C:41](=[O:49])[CH2:42][C:43]([CH3:47])([CH3:48])[C:44]([OH:46])=[O:45])[CH2:26][CH2:25]4)[CH2:22][CH2:21]2)[OH:17])=[CH:58][CH:59]=1
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 8471TriethylamineHCID 5003444Sodium cyanoborohydrideHCID 13908802(Dimethylamino)acetaldehyde--hydrogen chloride (1/1)HCID 86690378HCID 86690378、化合物

生成物 1

HCID 71580991Gsk-2838232収率 67.9%

試薬・触媒・溶媒 4

HCID 887
Methanol
溶媒
2 回
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒
HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a solution of 2-(dimethylamino)acetaldehyde, hydrochloride (6.75 g, 54.6 mmol) in methanol (20 mL) was added 4-(((3aR,5aR,5bR,7aR,9S,11aR,11bR,13aS)-3a-((R)-2-((4-chlorobenzyl)amino)-1-hydroxyethyl)-1-isopropyl-5a,5b,8,8,11a-pentamethyl-2-oxo-3,3a,4,5,5a,5b,6,7,7a,8,9,10,11,11a,11b,12,13,13a-octadecahydro-2H-cyclopenta[a]chrysen-9-yl)oxy)-2,2-dimethyl-4-oxobutanoic acid, Trifluoroacetic acid salt (46) (9.5 g, 10.92 mmol). The pH was adjusted to 7-8 with Et3N. The reaction mixture was stirred at rt for 2 h. Sodium cyanoborohydride (0.686 g, 10.92 mmol) was then added and the mixture was stirred at rt overnight. After the reaction was complete, water (15 mL) and EtOAc (15 mL) were added, and then the organic phase was removed and concentrated under reduced pressure. The product was extracted with EtOAc (80 mLx3), the combined organic phase was washed with brine, dried, and concentrated. The product was purified by flash chromatography (DCM:EtOAc=2:1 to 1:1, then DCM:MeOH=100:1 to 20:1) to give 4-(((3aR,5aR,5bR,7aR,9S,11aR,11bR,13aS)-3a-((R)-2-((4-chlorobenzyl)(2-(dimethylamino)ethyl)amino)-1-hydroxyethyl)-1-isopropyl-5a,5b,8,8,11a-pentamethyl-2-oxo-3,3a,4,5,5a,5b,6,7,7a,8,9,10,11,11a,11b,12,13,13a-octadecahydro-2H-cyclopenta[a]chrysen-9-yl)oxy)-2,2-dimethyl-4-oxobutanoic acid (51) (6 g, 7.41 mmol, 67.9% yield) as white solid. Multiple batches of this material (were combined 95 g), dissolved in 600 mL of dichloromethane and washed with NaHCO3 (400 mL*3) and the organic phase was dried over Na2SO4, filtered and concentrated. The solids were washed with a mixture of EtOAc: petroleum ether (600 mL), and filtered followed by lyophilization to provide the final title compound 62 g as a white solid. 1H NMR (400 MHz, METHANOL-d4) δ=7.47-7.29 (m, 4H), 4.48 (dd, J=5.8, 10.3 Hz, 1H), 4.15-4.04 (m, 1H), 3.80 (d, J=13.8 Hz, 1H), 3.57 (d, J=14.1 Hz, 1H), 3.21-2.82 (m, 5H), 2.72-2.41 (m, 9H), 2.37-2.05 (m, 4H), 2.05-0.74 (m, 45H);

後処理

  1. stirringthe mixture was stirred at rt overnight
  2. customthe organic phase was removed
  3. concentrationconcentrated under reduced pressure
  4. extractionThe product was extracted with EtOAc (80 mLx3)
  5. washthe combined organic phase was washed with brine
  6. customdried
  7. concentrationconcentrated
  8. customThe product was purified by flash chromatography (DCM

出典と根拠

ORDレコード
ord-02ac53cb1363427a90adea7cc1047652
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09102685B2

反応ノート

読み込み中…

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