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N'-Hydroxy-2-methylpropanimidamide → HCID 67125514, 화합물

HRID 1470765
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HRID 1470765 반응식
[C:1]([N:3]1[CH2:8][CH2:7][CH:6]([C:9]2[CH:14]=[CH:13][C:12]([C@@H:15]([NH:17][C:18](=[O:20])[CH3:19])[CH3:16])=[CH:11][CH:10]=2)[CH2:5][CH2:4]1)#[N:2].[OH:21][N:22]=[C:23](N)[CH:24]([CH3:26])[CH3:25]>C(OC(=O)C)C.[Cl-].[Zn+2].[Cl-]>[CH:24]([C:23]1[N:2]=[C:1]([N:3]2[CH2:8][CH2:7][CH:6]([C:9]3[CH:10]=[CH:11][C:12]([C@@H:15]([NH:17][C:18](=[O:20])[CH3:19])[CH3:16])=[CH:13][CH:14]=3)[CH2:5][CH2:4]2)[O:21][N:22]=1)([CH3:26])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2794833N'-Hydroxy-2-methylpropanimidamideHCID 86666703HCID 86666703, 화합물

생성물 1

HCID 67125514HCID 67125514, 화합물

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 8857Ethyl Acetate용매

실험 절차

0.9 mL (0.45 mmol) Zinc(II)chloride (0.5 M solution in THF) is added dropwise to a mixture of 40.7 mg (0.15 mmol) (S)—N-{1-[4-(1-cyano-piperidin-4-yl)-phenyl]-ethyl}-acetamide (XXVII.1) and 30.6 mg (0.30 mmol N′-hydroxy-2-methylpropanimidamide in 12 mL ethylacetate. The mixture is stirred for 12 h at rt. After that the solvent is removed in vacuo and 15 mL ethanol and 2 mL conc. HCl solution are added. The mixture is refluxed for 3 h. Subsequently the mixture is concentrated, water is added and the precipitate is collected and washed with water to yield the desired product.

후처리

  1. customAfter that the solvent is removed in vacuo and 15 mL ethanol and 2 mL conc. HCl solution
  2. additionare added
  3. temperatureThe mixture is refluxed for 3 h
  4. concentrationSubsequently the mixture is concentrated
  5. additionwater is added
  6. customthe precipitate is collected
  7. washwashed with water

출처 및 근거

ORD 기록
ord-0a5e82c0c18a4dacb690762dbbc03476
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006450B2

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