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1,2-Dichloroethane → 3-(trans-3-Cyclopropylmethoxytetrahydrofuran-4-ylamino)-6-chloro-1-(3-chloro-7-azaindol-5-ylmethylaminocarbonylmethyl)pyrazinone

HRID 398395
ノート
印刷プレビュー

反応式

HRID 398395 の反応式
[CH:1]1([CH2:4][O:5][C@H:6]2[C@H:10]([NH:11][C:12]3[C:13](=[O:23])[N:14]([CH2:19][C:20]([OH:22])=O)[C:15]([Cl:18])=[CH:16][N:17]=3)[CH2:9][O:8][CH2:7]2)[CH2:3][CH2:2]1.Cl.Cl.[NH2:26][CH2:27][C:28]1[CH:29]=[C:30]2[C:34](=[N:35][CH:36]=1)[NH:33][CH:32]=[C:31]2[Cl:37].C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C.C(Cl)CCl.CO>CN(C=O)C.Cl>[CH:1]1([CH2:4][O:5][C@H:6]2[C@H:10]([NH:11][C:12]3[C:13](=[O:23])[N:14]([CH2:19][C:20]([NH:26][CH2:27][C:28]4[CH:29]=[C:30]5[C:34](=[N:35][CH:36]=4)[NH:33][CH:32]=[C:31]5[Cl:37])=[O:22])[C:15]([Cl:18])=[CH:16][N:17]=3)[CH2:9][O:8][CH2:7]2)[CH2:2][CH2:3]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 6

HCID 111,2-DichloroethaneHCID 887MethanolHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 230002415-Aminomethyl-3-chloro-7-azaindole bis-hydrochloride saltHCID 700236133-(trans-3-Cyclopropylmethoxytetrahydrofuran-4-ylamino)-6-chloro-1-carboxymethylpyrazinone

生成物 1

HCID 70023399
3-(trans-3-Cyclopropylmethoxytetrahydrofuran-4-ylamino)-6-chloro-1-(3-chloro-7-azaindol-5-ylmethylaminocarbonylmethyl)pyrazinone

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of 3-(trans-3-cyclopropylmethoxytetrahydrofuran-4-ylamino)-6-chloro-1-carboxymethylpyrazinone from step 7 above (50 mg, 0.15 mmol) in DMF (1.0 mL) was added 5-aminomethyl-3-chloro-7-azaindole bis-hydrochloride salt (41 mg, 0.16 mmol) and HOBT (24 mg, 0.16 mmol). The solution was brought to pH 7 by the addition of DIEA (approximately 0.1 mL). EDC (70 mg, 0.24 mmol) was added and the solution was stirred at ambient temperature for 18 h. The reaction was concentrated in vacuo and partitioned between water and EtOAc. The organic phase was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash column chromatography using 9:1 CH2Cl2:MeOH as eluant. The free base of the title compound was dissolved in MeOH containing 3 equivalents of aqueous HCl and the solution was evaporated in vacuo to give the HCl salt of the title compound as an amorphous solid (45 mg, TLC Rf=0.46, 92:8:0.4 CH2Cl2:MeOH:NH4OH; HPLC RT=8.6 min, method A; M+1 peak at m/z=508, electrospray mass spec).

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. custompartitioned between water and EtOAc
  3. dry with materialThe organic phase was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash column chromatography

出典と根拠

ORDレコード
ord-9b8a72e5e81c41d9912a51af8d36b2f7
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06610692B1

反応ノート

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