Ammonia → HCID 86682396、化合物

HRID 1521749ノート

反応式

HRID 1521749 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH3:10])[C:5]([NH2:11])=[CH:4][CH:3]=1.[N:12]#[C:13]Br.C(Cl)Cl.N>C(O)C.CO>[Cl:1][C:2]1[N:7]=[C:6]2[N:8]([CH2:9][CH3:10])[C:13]([NH2:12])=[N:11][C:5]2=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 222AmmoniaHCID 6344DichloromethaneHCID 10476Cyanogen BromideHCID 10797271HCID 10797271、化合物

生成物 1

HCID 86682396HCID 86682396、化合物収率 46%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

To a solution of 6-chloro-N˜2˜-ethylpyridine-2,3-diamine (401 mg, 2.34 mmol) in ethanol (10 mL) is added a 3M solution of cyanogen bromide in CH2Cl2 (0.93 mL, 2.8 mmol) and the resulting solution is stirred for 6 h at room temperature. The solution is basified with ammonia in methanol and evaporated. The residue is purified via flash column chromatography using a gradient elution of 0-15% CH2Cl2/methanol containing 1% NH4OH to afford the title compound (212 mg, 46%).

後処理

  1. customevaporated
  2. customThe residue is purified via flash column chromatography
  3. washa gradient elution of 0-15% CH2Cl2/methanol containing 1% NH4OH

出典と根拠

ORDレコード
ord-cb1fad4757844191a7355708cea06f7f
出典データセット
uspto-grants-2015_07
特許番号
US09073926B2

反応ノート

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