Dichloromethane → N-{3-[2-(3-Acetylamino-phenylamino)-pyrrolo[2,1-f][1,2,4]triazin-7-yl]-phenyl}-2,2-dimethyl-propionamide

HRID 1262136

反応式

HRID 1262136 の反応式
[CH3:1][C:2]([CH3:24])([CH3:23])[C:3]([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([C:12]2[N:20]3[C:15]([CH:16]=[N:17][C:18](SC)=[N:19]3)=[CH:14][CH:13]=2)[CH:7]=1)=[O:4].CSC1N=CC2=CC=C([C:36]3[CH:37]=[C:38]([NH2:42])[CH:39]=[CH:40][CH:41]=3)N2N=1.C(Cl)Cl.[CH2:46]([N:48](CC)CC)[CH3:47].CC(C)(C)C(Cl)=[O:56]>>[C:46]([NH:48][C:36]1[CH:37]=[C:38]([NH:42][C:18]2[N:17]=[CH:16][C:15]3=[CH:14][CH:13]=[C:12]([C:8]4[CH:7]=[C:6]([NH:5][C:3](=[O:4])[C:2]([CH3:24])([CH3:23])[CH3:1])[CH:11]=[CH:10][CH:9]=4)[N:20]3[N:19]=2)[CH:39]=[CH:40][CH:41]=1)(=[O:56])[CH3:47]

参加物

6

反応物 5

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 62493Pivaloyl chlorideHCID 667116972,2-Dimethyl-N-[3-(2-methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-phenyl]-propionamideHCID 667126823-(2-Methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-phenylamine

生成物 1

HCID 66712052N-{3-[2-(3-Acetylamino-phenylamino)-pyrrolo[2,1-f][1,2,4]triazin-7-yl]-phenyl}-2,2-dimethyl-propionamide

反応条件

温度
0 °C

実験手順

2,2-Dimethyl-N-[3-(2-methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-phenyl]-propionamide. 3-(2-Methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-phenylamine (0.200 g, 0.780 mmol) was dissolved in Methylene chloride (10.0 mL, 156 mmol) and cooled to 0° C. Triethylamine (0.130 mL, 0.936 mmol) was added followed by 2,2-Dimethylpropanoyl chloride (0.106 mL, 0.858 mmol). The reaction mixture was allowed to warm to rt. LCMS after 30 min indicated mass of title compound. Reaction mixture was washed with water, dried over MgSO4, filtered, and concentrated. HPLC rt=3.436, purity=90%, LCMS=341.2 (M+H).

後処理

  1. temperatureto warm to rt

出典と根拠

ORDレコード
ord-8331ea240a1343d298aa48c4930429c6
出典データセット
uspto-grants-2013_06
特許番号
US08471005B2

関連ノート

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