1-Methylpiperazine → HCID 136377200, 화합물

HRID 624546노트

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HRID 624546 반응식
Cl.[NH2:2][C:3]1[C:12]2[CH:11]=[C:10]([CH3:13])[S:9][C:8]=2[NH:7][C:6]2[CH:14]=[CH:15][C:16]([C:18]#[N:19])=[CH:17][C:5]=2[N:4]=1.[CH3:20][N:21]1[CH2:26][CH2:25]N[CH2:23][CH2:22]1>CS(C)=O.C1(C)C=CC=CC=1>[CH3:13][C:10]1[S:9][C:8]2[NH:7][C:6]3[CH:14]=[CH:15][C:16]([C:18]#[N:19])=[CH:17][C:5]=3[N:4]=[C:3]([N:2]3[CH2:25][CH2:26][N:21]([CH3:20])[CH2:22][CH2:23]3)[C:12]=2[CH:11]=1

참가 물질

5

반응물 2

HCID 531671-MethylpiperazineHCID 136377198HCID 136377198, 화합물

생성물 1

HCID 136377200HCID 136377200, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 1140Toluene용매

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온도
130 °C

실험 절차

To a solution of 10-amino-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulene-7-carbonitrile hydrochloride, prepared as described in the previous step, (0.6 g) in DMSO (6 mL) and toluene (6 mL), was added 1-methylpiperazine (4 mL). The mixture was heated in a 130° C. oil bath for 17 hours. The solution was concentrated, diluted with ethyl acetate (50 mL), washed with water (20 mL) and brine (20 mL), and then concentrated. The solid was dissolved in dichloromethane (10 mL) and treated with saturated sodium bicarbonate solution. The title compound was collected as a light yellow precipitate, washed with water and dichloromethane, dried, and used in the next step without additional purification. LC-MS: m/z 338 (M+1). 1H NMR (CD3OD, 400 MHz): δ (ppm) 7.19-7.15 (m, 2H), 6.74 (d, 1H), 6.37 (s, 1H), 3.51 (m, 4H), 2.53 (m, 4H), 2.34 (s, 3H), 2.32 (s, 3H).

후처리

  1. concentrationThe solution was concentrated
  2. additiondiluted with ethyl acetate (50 mL)
  3. washwashed with water (20 mL) and brine (20 mL)
  4. concentrationconcentrated
  5. dissolutionThe solid was dissolved in dichloromethane (10 mL)
  6. additiontreated with saturated sodium bicarbonate solution
  7. customThe title compound was collected as a light yellow precipitate
  8. washwashed with water and dichloromethane
  9. customdried
  10. customused in the next step without additional purification

출처 및 근거

ORD 기록
ord-8703ad7d687d450092b3cd5af6ec396a
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09303041B2

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