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Triethylamine → (S)-2-{[2-(2-1H-Indazol-4-yl-acetylamino)-4-methyl-thiazole-5-carbonyl]-amino}-3-[(thiophene-2-carbonyl)-amino]-propionic acid methyl ester

HRID 1952557
ノート
印刷プレビュー

反応式

HRID 1952557 の反応式
[CH3:1][O:2][C:3](=[O:42])[C@@H:4]([NH:14][C:15]([C:17]1[S:21][C:20]([NH:22][C:23](=[O:40])[CH2:24][C:25]2[CH:33]=[CH:32][CH:31]=[C:30]3[C:26]=2[CH:27]=[N:28][N:29]3C2CCCCO2)=[N:19][C:18]=1[CH3:41])=[O:16])[CH2:5][NH:6][C:7](OC(C)(C)C)=[O:8].O1[CH2:48][CH2:47]OCC1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C1C=CC2N(O)N=NC=2C=1.[S:83]1[CH:87]=CC=[C:84]1C(O)=O.C(N(CC)CC)C>Cl.CO>[CH3:1][O:2][C:3](=[O:42])[C@@H:4]([NH:14][C:15]([C:17]1[S:21][C:20]([NH:22][C:23](=[O:40])[CH2:24][C:25]2[CH:33]=[CH:32][CH:31]=[C:30]3[C:26]=2[CH:27]=[N:28][NH:29]3)=[N:19][C:18]=1[CH3:41])=[O:16])[CH2:5][NH:6][C:7]([C:84]1[S:83][CH:87]=[CH:47][CH:48]=1)=[O:8]
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 6

HCID 8471TriethylamineHCID 107002-Thiophenecarboxylic acidHCID 312751,4-DioxaneHCID 757711-HydroxybenzotriazoleHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 86671256
(S)-3-tert-Butoxycarbonylamino-2-[(4-methyl-2-{2-[1-(tetrahydro-pyran-2-yl)-1H-indazol-4-yl]-acetylamino}-thiazole-5-carbonyl)-amino]-propionic acid methyl ester

生成物 1

HCID 86671255(S)-2-{[2-(2-1H-Indazol-4-yl-acetylamino)-4-methyl-thiazole-5-carbonyl]-amino}-3-[(thiophene-2-carbonyl)-amino]-propionic acid methyl ester収率 42.9%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

実験手順

A solution of (S)-3-tert-Butoxycarbonylamino-2-[(4-methyl-2-{2-[1-(tetrahydro-pyran-2-yl)-1H-indazol-4-yl]-acetylamino}-thiazole-5-carbonyl)-amino]-propionic acid methyl ester (96.1 mg, 0.160 mmol) in 4M HCl in dioxane (4 mL, 16 mmol) was stirred at room temp for 40 min. Methanol (0.5 mL) was added to the gummy precipitate and the resulting solution was stirred at room temp for 5½ h. The reaction solution was concentrated under reduced pressure, added ether (2×) with concentrating under reduced pressure. To the resulting white solid dissolved in anhydrous DMF (3 mL) was added HBTU (91 mg, 0.240 mmol), HOBt (32 mg, 0.237 mmol), 2-thiophenecarboxylic acid (26 mg, 0.203 mmol) and triethylamine (0.12 mL, 0.861 mmol). The solution was allowed to stir at 25° C. for 1 h and concentrated under reduced pressure to remove most of the DMF. Ethyl acetate (80 mL) was added, washed with 3/1 water/brine (20 mL), aqueous 1N HCl (20 mL), brine (20 mL), dried over MgSO4, filtered and concentrated under reduced pressure. The resulting crude compound was purified by flash chromatography (50% to 100% EtOAc in hexanes) to give (S)-2-{[2-(2-1H-Indazol-4-yl-acetylamino)-4-methyl-thiazole-5-carbonyl]-amino}-3-[(thiophene-2-carbonyl)-amino]-propionic acid methyl ester (36.1 mg, 42.9%) as a white solid. MS m/e 527.6 (M+H+).

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionadded ether (2×)
  3. concentrationwith concentrating under reduced pressure
  4. dissolutionTo the resulting white solid dissolved in anhydrous DMF (3 mL)
  5. stirringto stir at 25° C. for 1 h
  6. concentrationconcentrated under reduced pressure
  7. customto remove most of the DMF
  8. additionEthyl acetate (80 mL) was added
  9. washwashed with 3/1 water/brine (20 mL), aqueous 1N HCl (20 mL), brine (20 mL)
  10. dry with materialdried over MgSO4
  11. filtrationfiltered
  12. concentrationconcentrated under reduced pressure
  13. customThe resulting crude compound was purified by flash chromatography (50% to 100% EtOAc in hexanes)

出典と根拠

ORDレコード
ord-832a91c73634491484e8ed2f7bf12b85
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08404859B2

反応ノート

読み込み中…

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