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Dimethylformamide → 2-Chloro-6H-thieno[2,3-b]pyrrole-5-carboxylic acid-[1-benzyl-2-methoxy-2-(methoxymethyl-carbamoyl)-ethyl]-amide

HRID 1612046
ノート
印刷プレビュー

反応式

HRID 1612046 の反応式
C(N(CC)CC)C.[NH2:8][CH:9]([CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH:10]([O:17][CH3:18])[C:11]([N:13](OC)[CH3:14])=[O:12].[Cl:26][C:27]1[S:37][C:30]2[NH:31][C:32]([C:34](O)=[O:35])=[CH:33][C:29]=2[CH:28]=1.C1C=CC2N(O)N=NC=2C=1.CN([CH:51]=[O:52])C>C(OCC)(=O)C>[CH2:19]([CH:9]([NH:8][C:34]([C:32]1[NH:31][C:30]2[S:37][C:27]([Cl:26])=[CH:28][C:29]=2[CH:33]=1)=[O:35])[CH:10]([O:17][CH3:18])[C:11](=[O:12])[NH:13][CH2:14][O:52][CH3:51])[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 6228Dimethylformamide2 回HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 104428202-Chloro-6H-thieno[2,3-b]pyrrole-5-carboxylic acidHCID 222529473-amino-2,N-dimethoxy-N-methyl-4-phenyl-butyramide

生成物 1

HCID 22252951
2-Chloro-6H-thieno[2,3-b]pyrrole-5-carboxylic acid-[1-benzyl-2-methoxy-2-(methoxymethyl-carbamoyl)-ethyl]-amide

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Triethylamine was added dropwise to a solution of 3-amino-2,N-dimethoxy-N-methyl-4-phenyl-butyramide (PCT International Application Publication No. WO 96/39385) (1.65 g, 5.71 mmol) in DMF (15 mL) and cooled in an ice bath. A solution of 2-chloro-6H-thieno[2,3-b]pyrrole-5-carboxylic acid (U.S. Pat. No. 6,399,601) (1.1 g, 5.71 mmol) in 15 mL of DMF was added dropwise followed by the addition of HOBT (1.16 g, 11.4 mmol) neat. The reaction mixture was stirred for 5 min and N-ethyliminomethylene-N,N′-dimethyl-propane-1,3-diamine (1.10 g, 5.71 mmol) was added neat. The resulting mixture was stirred at room temperature for 18 hrs. The reaction mixture was diluted with ethyl acetate (150 mL) and washed with saturated ammonium chloride, water, and brine. The ethyl acetate was dried and evaporated in vacuo to yield 2.54 g of crude product. Chromatography over silica gel, eluting with ethyl acetate/hexanes (1:2), afforded 1.43 g of the title compound.

後処理

  1. stirringThe resulting mixture was stirred at room temperature for 18 hrs
  2. washwashed with saturated ammonium chloride, water, and brine
  3. dry with materialThe ethyl acetate was dried
  4. customevaporated in vacuo
  5. customto yield 2.54 g of crude product
  6. washChromatography over silica gel, eluting with ethyl acetate/hexanes (1:2)

出典と根拠

ORDレコード
ord-9c08440f20d54915aa9e7039f4f49833
出典データセット
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06992101B2

反応ノート

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