Potassium Carbonate → HCID 21886024, 화합물

HRID 722718노트

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HRID 722718 반응식
[NH2:1][C:2]1[S:10][C:5]2[CH2:6][O:7][CH2:8][CH2:9][C:4]=2[C:3]=1[C:11]#[N:12].C(=O)([O-])[O-].[K+].[K+].[C:19]1([CH:25]([CH2:29][CH3:30])[C:26](Cl)=[O:27])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(OCC)C>[C:11]([C:3]1[C:4]2[CH2:9][CH2:8][O:7][CH2:6][C:5]=2[S:10][C:2]=1[NH:1][C:26](=[O:27])[CH:25]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:29][CH3:30])#[N:12]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 981732-Phenylbutyryl chlorideHCID 7377432-Amino-4,7-dihydro-5H-thieno[2,3-c]pyran-3-carbonitrile

생성물 1

HCID 21886024HCID 21886024, 화합물수율 66%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a stirred suspension of 2-Amino-3-cyano-4,7-dihydro-5H-thieno[2,3-c]pyran (361 mg; 2.0 mmol; prepared as described in Example 2, Step 1) and potassium carbonate (1.40 g; 10.1 mmol) in diethylether (6.0 mL) was added 2-phenylbutyryl chloride dropwise. The resulting mixture was stirred at room temperature for 24 h. The solvent was then removed in vacuo, the residue taken up into methylene chloride and washed with water. The organic layer was dried (sodium sulfate) filtered and concentrated in vacuo to give crude product which was triturated with diethyl ether to provide 428 mg (66%) of N-(3-Cyano-4,7-dihydro-5H-thieno[2,3-c]pyran-2-yl)-2-phenyl-butyramide as a beige colored solid. EI-HRMS m/e calcd for C18H18N2O2S (M+) 326.1809, found 326.1809.

후처리

  1. customThe solvent was then removed in vacuo
  2. washwashed with water
  3. dry with materialThe organic layer was dried (sodium sulfate)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto give crude product which
  7. customwas triturated with diethyl ether

출처 및 근거

ORD 기록
ord-ef1f2603911e4bc387d6d70d1eb54c6b
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138529B2

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