5-(Bromomethyl)-1-methyl-1H-benzotriazole → HCID 67219816、化合物

HRID 1445626ノート

反応式

HRID 1445626 の反応式
[CH3:1][O:2][C:3](=[O:15])[CH2:4][C:5]1[C:13]2[C:8](=[N:9][CH:10]=[CH:11][CH:12]=2)[NH:7][C:6]=1[CH3:14].[CH3:16]CN(P1(N(C)CCCN1C)=NC(C)(C)C)CC.BrC[C:36]1[CH:45]=[CH:44][C:39]2[N:40]([CH3:43])[N:41]=[N:42][C:38]=2[CH:37]=1>CN(C=O)C>[CH3:1][O:2][C:3](=[O:15])[CH2:4][C:5]1[C:13]2[C:8](=[N:9][CH:10]=[CH:11][CH:12]=2)[N:7]([CH2:16][C:45]2[CH:36]=[CH:37][C:38]3[N:42]=[N:41][N:40]([CH3:43])[C:39]=3[CH:44]=2)[C:6]=1[CH3:14]

参加物

5

反応物 3

HCID 27954185-(Bromomethyl)-1-methyl-1H-benzotriazoleHCID 35138512-((1,1-Dimethylethyl)imino)-N,N-diethylhexahydro-1,3-dimethyl-2lambda5-1,3,2-diazaphosphorin-2-amineHCID 67218699methyl 2-(2-methyl-1H-pyrrolo[2,3-b]pyridin-3-yl)acetate

生成物 1

HCID 67219816HCID 67219816、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of (2-methyl-1H-pyrrolo[2,3-b]pyridin-3-yl)-acetic acid methyl ester ((0.025 g, 0.122 mmol) in dry DMF (1 ml) under an inert atmosphere of Argon is added dropwise, BEMP (56.6 μl, 0.196 mmol). The mixture is agitated at room temperature for 1 hour before cooling to 0° C. with an ice-bath. A solution of 5-bromomethyl-1-methyl-1H-benzotriazole (0.044 g, 0.196 mmol) in DMF (1 ml) is added to the cooled solution and the resulting mixture is agitated at room temperature for 2 days. The solvent is removed in vacuo and purification of the crude by chromatography on silica eluting with iso-hexane/ethyl acetate (0%-20% ethyl acetate) yields the titled product. (MH+ 350).

後処理

  1. temperaturebefore cooling to 0° C. with an ice-bath
  2. stirringthe resulting mixture is agitated at room temperature for 2 days
  3. customThe solvent is removed in vacuo and purification of the crude by chromatography on silica eluting with iso-hexane/ethyl acetate (0%-20% ethyl acetate)

出典と根拠

ORDレコード
ord-4142e9ba9313453182e20849e112de67
出典データセット
uspto-grants-2010_02
特許番号
US07666878B2

反応ノート

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