Benzylamine → HCID 178508735、化合物

HRID 555921ノート

反応式

HRID 555921 の反応式
Cl[C:2]1[N:7]=[C:6]([NH2:8])[C:5]([C:9]2[NH:13][N:12]=[N:11][N:10]=2)=[CH:4][N:3]=1.CCN(C(C)C)C(C)C.[CH2:23]([NH2:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>O1CCOCC1>[CH2:23]([NH:30][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([C:9]2[NH:13][N:12]=[N:11][N:10]=2)=[CH:4][N:3]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

5

反応物 3

HCID 7504BenzylamineHCID 81531DiisopropylethylamineHCID 1785084532-Chloro-5-(1H-tetrazol-5-yl)pyrimidin-4-amine

生成物 1

HCID 178508735HCID 178508735、化合物収率 10.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

In a microwave tube, 2-chloro-5-(1H-tetrazol-5-yl)pyrimidin-4-amine (200 mg, 1.0 mmol) was dissolved into 3 mL of dioxane and DIPEA (1.5 mmol, 1.5 eq.). After the addition of benzylamine (5.0 mmol, 5.0 eq.), the tube was capped and irradiated in a CEM Discover microwave reactor to 120° C. for a total of 60 minutes in three 20 minutes intervals. LC/MS was taken every 20 minutes to follow the disappearance of starting material. After the complete consumption of the starting material, the reaction was cooled to room temperature and a precipitate formed. This solid was collected by filtration, washed several times with water, then with hot EtOAc. It was dried under vacuum to afford 27 mg of desired product. This material was carried forward without further purification. MS (EI) for C12H12N8: 269 (M+H).

後処理

  1. customthe tube was capped
  2. customirradiated in a CEM Discover microwave reactor to 120° C. for a total of 60 minutes in three 20 minutes intervals
  3. customAfter the complete consumption of the starting material
  4. customa precipitate formed
  5. filtrationThis solid was collected by filtration
  6. washwashed several times with water
  7. customIt was dried under vacuum

出典と根拠

ORDレコード
ord-ae219e88bfab4212aac734d71344c1e0
出典データセット
uspto-grants-2011_11
特許番号
US08053454B2

反応ノート

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