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Dichloromethane → HSD Inhibitor 23

HRID 386518
ノート
印刷プレビュー

反応式

HRID 386518 の反応式
[CH3:1][C:2]([N:7]1[CH2:12][CH2:11][N:10]([C:13]2[CH:18]=[CH:17][C:16]([C:19]([F:22])([F:21])[F:20])=[CH:15][N:14]=2)[CH2:9][CH2:8]1)([CH3:6])[C:3](O)=[O:4].O.[OH:24][C:25]1[C:33]2N=NN[C:29]=2[CH:28]=[CH:27][CH:26]=1.Cl.CN(C)[CH2:37][CH2:38][CH2:39][N:40]=C=NCC.[CH2:46](Cl)Cl>CCN(C(C)C)C(C)C>[CH3:6][C:2]([N:7]1[CH2:8][CH2:9][N:10]([C:13]2[CH:18]=[CH:17][C:16]([C:19]([F:20])([F:22])[F:21])=[CH:15][N:14]=2)[CH2:11][CH2:12]1)([C:3]([NH:40][CH:39]1[CH:27]2[CH2:26][C:25]3([OH:24])[CH2:37][CH:38]1[CH2:46][CH:29]([CH2:33]3)[CH2:28]2)=[O:4])[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6344Dichloromethane2 回HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 16100379HCID 16100379、化合物HCID 178526939HCID 178526939、化合物

生成物 1

HCID 11634114HSD Inhibitor 23

試薬・触媒・溶媒 1

HCID 81531
Diisopropylethylamine
溶媒

実験手順

A solution of 2-methyl-2-[4-(5-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-propionic acid (159 mg, 0.5 mmoles) from Example 14C in DCM (5 mL) and DIPEA (0.5 mL) was treated with hydroxybenzotriazole hydrate (HOBt) (84 mg, 0.6 mmoles), 5-hydroxy-2-adamantamine (100 mg, 0.6 mmoles) from Example 13A and 15 minutes later with (3-dimethylaminopropyl)-3-ethylcarbodiimide HCl (EDCI) (115 mg, 0.6 mmoles). The mixture was stirred overnight at room temperature after which the DCM was removed under reduced pressure and the residue was partitioned between water and ethyl acetate. The aqueous layer was extracted with ethyl acetate and the combined organic extracts washed with saturated sodium bicarbonate, water, dried (MgSO4) and filtered. The filtrate was concentrated under reduced pressure and the crude product purified (silica gel, 10-40% acetone in hexane) to provide the title compound as a white solid. 1H NMR (300 MHz, CDCl3) δ 8.41 (s, 1H), 7.67 (m, 2H), 6.66 (d, J=9.1 Hz, 1H), 4.0 (d, J=7.8 Hz, 1H), 3.66 (m, 4H), 2.64 (m, 4H), 2.23-2.1 (m, 3H), 1.9-1.63 (m, 10H), 1.25 (s, 6H); MS (APCI+) m/z 467 (M+H)+.

後処理

  1. customwas removed under reduced pressure
  2. customthe residue was partitioned between water and ethyl acetate
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. washthe combined organic extracts washed with saturated sodium bicarbonate, water
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customthe crude product purified (silica gel, 10-40% acetone in hexane)

出典と根拠

ORDレコード
ord-b97e294af9714a44b23253929576cc63
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08372841B2

反応ノート

読み込み中…

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