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Ammonia → HCID 66571317, 화합물

HRID 924685
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HRID 924685 반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[NH:11][C:10]([C:12]3[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:13]=3[CH3:19])=[C:9]([C:20]#[N:21])[CH:8]=2)=[N:3][CH:2]=1.O.S(=O)(=O)(O)[OH:24].N>C(O)(C(F)(F)F)=O>[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[NH:11][C:10]([C:12]3[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:13]=3[CH3:19])=[C:9]([C:20]([NH2:21])=[O:24])[CH:8]=2)=[N:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 962Water2회HCID 1118Sulfuric AcidHCID 70979552HCID 70979552, 화합물

생성물 1

HCID 66571317HCID 66571317, 화합물수율 83%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

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온도
70 °C

실험 절차

To a solution of 5-(pyrimidin-4-yl)-2-(5-chloro-2-methyl-phenyl)-1H-pyrrole-3-carbonitrile (85 mg, 0.28 mmol) in TFA (1.0 mL) were sequentially added water (0.15 mL) and 98% sulfuric acid (0.30 mL) under efficient stirring. The mixture was allowed to stir for 5 h at 70° C. and then was diluted by drop wise addition of water (1 mL). The reaction mixture was made basic (pH 10-12) by adding 30% aqueous ammonia (3 mL) under stirring. The precipitated solid was collected by filtration, washed with water and finally dried in a vacuum oven at 50° C. affording the title compound (72 mg, 83%).

후처리

  1. stirringunder stirring
  2. filtrationThe precipitated solid was collected by filtration
  3. washwashed with water
  4. customfinally dried in a vacuum oven at 50° C.

출처 및 근거

ORD 기록
ord-9a752a74d7fb4a17bfba4f6950c3531f
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09283224B2

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