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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 1-[[(3S)-3-[[2-[(3-thienyl)sulfonyl]-2-cyano-1-[(2-methyl-5-benzofuranyl)amino]-1-ethenyl]amino]hexahydro-2-oxo-1H-azepin-1-yl]acetyl]pyrrolidine

HRID 1264640
ノート
印刷プレビュー

反応式

HRID 1264640 の反応式
[S:1]1[CH:5]=[CH:4][C:3]([S:6]([CH2:9][C:10]#[N:11])(=[O:8])=[O:7])=[CH:2]1.[H-].[Na+].[N:14]([C:17]1[CH:18]=[CH:19][C:20]2[O:24][C:23]([CH3:25])=[CH:22][C:21]=2[CH:26]=1)=[C:15]=S.[NH2:27][C@H:28]1[CH2:34][CH2:33][CH2:32][CH2:31][N:30]([CH2:35][C:36]([N:38]2[CH2:42][CH2:41][CH2:40][CH2:39]2)=[O:37])[C:29]1=[O:43].CCN=C=NCCCN(C)C>CN(C=O)C.CN(C)C1C=CN=CC=1.O>[S:1]1[CH:5]=[CH:4][C:3]([S:6]([C:9]([C:10]#[N:11])=[C:15]([NH:27][C@H:28]2[CH2:34][CH2:33][CH2:32][CH2:31][N:30]([CH2:35][C:36]([N:38]3[CH2:39][CH2:40][CH2:41][CH2:42]3)=[O:37])[C:29]2=[O:43])[NH:14][C:17]2[CH:18]=[CH:19][C:20]3[O:24][C:23]([CH3:25])=[CH:22][C:21]=3[CH:26]=2)(=[O:8])=[O:7])=[CH:2]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 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 24758Sodium hydrideHCID 27975192-(3-Thienylsulfonyl)acetonitrileHCID 120478195-Isothiocyanato-2-methylbenzofuranHCID 12047820(S)-1-[(3-amino-hexahydro-2-oxo-1H-azepin-1-yl)acetyl]pyrrolidine

生成物 1

HCID 69984479
1-[[(3S)-3-[[2-[(3-thienyl)sulfonyl]-2-cyano-1-[(2-methyl-5-benzofuranyl)amino]-1-ethenyl]amino]hexahydro-2-oxo-1H-azepin-1-yl]acetyl]pyrrolidine
収率 41%

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of (3-thienylsulphonyl)acetonitrile (59.4 mg, 0.318 mmol) in DMF (1 mL) was added NaH (95%, 8.08 mg, 0.344 mmol). After stirring 5 min at room temperature, 5-isothiocyanato-2-methylbenzofuran (50 mg, 0.265 mmol) was added in one portion. The reaction was heated at 50° C. for 30 min. To the mixture was added 1-[[(3S)-3-aminohexahydro-2-oxo-1H-azepin-1-yl]acetyl]pyrrolidine (76.0 mg, 0.318 =mol), WSC (101.7 mg, 0.53 mmol) and N,N-dimethyl 4-pyridinamine (cat.) in that order. The reaction mixture was stirred at room temperature overnight. Water was added to the reaction and the mixture was extracted with ethyl acetate three times. The combined organic fractions were washed once with brine, dried over magnesium sulfate and evaporated. The residue was chromatographed (silica, 5% methanol/ethyl acetate) to provide 1-[[(3S)-3-[[2-[(3-thienyl)sulfonyl]-2-cyano-1-[(2-methyl-5-benzofuranyl)amino]-1-ethenyl]amino]hexahydro-2-oxo-1H-azepin-1-yl]acetyl]pyrrolidine (63.0 mg, 41%): HPLC (method A) tR 3.65 min; LRMS (ESI, pos. ion spectrum) m/z 582 (M+H).

後処理

  1. temperatureThe reaction was heated at 50° C. for 30 min
  2. stirringThe reaction mixture was stirred at room temperature overnight
  3. extractionthe mixture was extracted with ethyl acetate three times
  4. washThe combined organic fractions were washed once with brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customThe residue was chromatographed (silica, 5% methanol/ethyl acetate)

出典と根拠

ORDレコード
ord-6b94f901fb3046edb2fc1bbd2d45e38b
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06544981B2

反応ノート

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