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Sodium Sulfide → HCID 178508202, 화합물

HRID 536236
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인쇄 미리보기

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HRID 536236 반응식
Br.C[O:3][C:4]1[CH:5]=[CH:6][C:7]2[C:8]3[N:9]([CH2:15][CH2:16][N:17]=3)[C:10]([NH2:14])=[N:11][C:12]=2[CH:13]=1.[S-2].[Na+].[Na+]>CN1CCCC1=O>[NH2:14][C:10]1[N:9]2[CH2:15][CH2:16][N:17]=[C:8]2[C:7]2[CH:6]=[CH:5][C:4]([OH:3])=[CH:13][C:12]=2[N:11]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14804Sodium SulfideHCID 178419595CID 67338391

생성물 1

HCID 178508202HCID 178508202, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
160 °C

실험 절차

8-Methoxy-2,3-dihydroimidazo[1,2-c]quinazolin-5-amine (Step 3, 1.00 g, 0.002 mol) was dissolved in 1-methyl-2-pyrrolidinone (20 ml) and treated with sodium sulfide (0.76 g, 0.010 mol) and heated to 160° C. for 5 h. It was cooled, filtered from reaction rinsing with EtOAc. The solid was dissolved in a minimal amount of water and brought to pH=1 with 2N HCl, then back to pH=7 with 1N NaOH and filtered.

후처리

  1. temperatureIt was cooled
  2. filtrationfiltered from reaction
  3. washrinsing with EtOAc
  4. dissolutionThe solid was dissolved in a minimal amount of water
  5. filtrationback to pH=7 with 1N NaOH and filtered

출처 및 근거

ORD 기록
ord-194a98ff71dd40aaaa850a56545bf770
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859572B2

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