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Methylamine → HCID 57708177, 화합물

HRID 643716
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HRID 643716 반응식
[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([C:17]([CH3:21])([CH3:20])[CH2:18][NH2:19])(=[O:16])=[O:15])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:3][CH2:2]1.[CH2:27]([N:29]([CH2:32]C)CC)C.ClC(OC1C=CC([N+]([O-])=O)=CC=1)=[O:36].CN.[OH-].[Na+]>ClCCl.C(OCC)(=O)C>[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([C:17]([CH3:20])([CH3:21])[CH2:18][NH:19][C:27]([NH:29][CH3:32])=[O:36])(=[O:16])=[O:15])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:2][CH2:3]1
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반응물 5

HCID 6329MethylamineHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 821294-Nitrophenyl chloroformateHCID 68615718HCID 68615718, 화합물

생성물 1

HCID 57708177HCID 57708177, 화합물수율 17%

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-{[1-(cyclopropylmethyl)-2-(2,2-dimethylpropyl)-1H-benzimidazol-5-yl]sulfonyl}-2-methylpropan-1-amine (Step K of Example 13, 177 mg, 0.469 mmol) and triethylamine (131 μL, 0.938 mmol) in dichloromethane (4 mL) was added p-nitrophenyl chloroformate (104 mg, 0.516 mmol) at room temperature. After stirring for 30 min, methylamine (40% aqueous solution, 3 mL) was added to the mixture and the whole was stirred for 2 h. To the resulting mixture was added ethyl acetate and 2 mol/L sodium hydroxide aqueous solution. The organic layer was dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by HPLC (ODS, gradient elution with Acetonitrile 10.01% aq. NH3=4:96 to 96:4, by volume; flow rate 40 mL/min) to afford the title compound (34 mg, 17%) as an amorphous.

후처리

  1. stirringthe whole was stirred for 2 h
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by HPLC (ODS, gradient elution with Acetonitrile 10.01% aq. NH3=4:96 to 96:4, by volume; flow rate 40 mL/min)

출처 및 근거

ORD 기록
ord-7a60c0196f5a45d38896224a7c44494e
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07700618B2

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