5-(Bromomethyl)-1-methyl-1H-benzotriazole → HCID 67219816, 화합물

HRID 1631498노트

반응식

HRID 1631498 반응식
[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]

참가 물질

5

반응물 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

생성물 1

HCID 67219816HCID 67219816, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-5214433ff6c246e9b5c1f9d7671fa1b7
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08791256B2

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