Acetonitrile → 2-[4-(4-Benzyl-phthalazin-1-yl)-piperazin-1-yl]-pyrimidine-5-carbonitrile

HRID 42185

반응식

HRID 42185 반응식
[CH2:1]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[N:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:25]1[N:30]=[CH:29][C:28]([C:31]#[N:32])=[CH:27][N:26]=1.CC#N>CN1C(=O)CCC1>[CH2:1]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([N:18]2[CH2:23][CH2:22][N:21]([C:25]3[N:30]=[CH:29][C:28]([C:31]#[N:32])=[CH:27][N:26]=3)[CH2:20][CH2:19]2)=[N:10][N:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 64040231-Benzyl-4-piperazin-1-yl-phthalazineHCID 214735922-Chloro-5-pyrimidinecarbonitrile

생성물 1

HCID 250646652-[4-(4-Benzyl-phthalazin-1-yl)-piperazin-1-yl]-pyrimidine-5-carbonitrile

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

Using the general protocol, 1-benzyl-4-piperazin-1-yl-phthalazine (56 mg, 0.184 mmol) and 2-chloro-5-cyanopyrimidine (44.5 mg, 0.239 mmol) are added into a microwave vial, equipped with a stir bar, and MeCN (0.5 ml) and NMP (0.5 ml) are dispensed. The vial is sealed and the reaction was irradiated at high level absorption in the microwave at 180° C. for 15 min. The product is observed as the main peak (m/z; M+1=408). The compound is purified by preparative HPLC using a C8-254 nm method.

후처리

  1. additionare added into a microwave vial
  2. customequipped with a stir bar
  3. customThe vial is sealed
  4. customthe reaction was irradiated at high level absorption in the microwave at 180° C. for 15 min
  5. customThe compound is purified by preparative HPLC

출처 및 근거

ORD 기록
ord-77371620f1054379bec421fa4520ef0c
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536168B2

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