HCID 67199810、化合物 → HCID 86621654、化合物

HRID 1711382ノート

反応式

HRID 1711382 の反応式
[ClH:1].[NH2:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([NH:16]C(=O)C)=[CH:12][CH:11]=2)[CH:6]=[C:5]([CH3:20])[N:4]=1>Cl>[ClH:1].[NH2:16][C:13]1[CH:12]=[CH:11][C:10]([NH:9][C:7]2[CH:6]=[C:5]([CH3:20])[N:4]=[C:3]([NH2:2])[N:8]=2)=[CH:15][CH:14]=1

参加物

3

反応物 1

HCID 67199810HCID 67199810、化合物

生成物 1

HCID 86621654HCID 86621654、化合物収率 99.3%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

To a suspension of 16 (6.0 g, 20 mmol) was added 2N HCl (40 mL) and the mixture was refluxed for 20 h. The solvents were evaporated to dryness, residue boiled in MeOH and diluted with EtOAc. The resulting precipitate was filtered and washed with EtOAc and dried to give essentially pure 17 (5.0 g, 97%); mp (MeOH/EtOAc) 275-280° C.; 1H NMR [(CD3)2SO] δ 12.50 (br, 1H, N+H), 10.75 (br s, 1H, NH), 9.75 (br s, 2H, NH2), 7.85 (br s, 4H, NH2 & ArH)), 7.34 (d, J=8.6 Hz, 2H, ArH), 6.24 (br s, 1H, ArH), 2.79 (s, 3H, CH3), HRMS (FAB+) calc. for C11H14N5 (M+1) m/z 216.1249, found 216.1247.

後処理

  1. temperaturethe mixture was refluxed for 20 h
  2. customThe solvents were evaporated to dryness, residue
  3. additiondiluted with EtOAc
  4. filtrationThe resulting precipitate was filtered
  5. washwashed with EtOAc
  6. customdried

出典と根拠

ORDレコード
ord-ee4cb32609a14141abd2a69cdf555849
出典データセット
uspto-grants-2010_09
特許番号
US07790746B2

反応ノート

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