Methyl iodide → HCID 66634917、化合物

HRID 510070ノート

反応式

HRID 510070 の反応式
[CH3:1][O:2][C:3]1[CH:38]=[C:37]([O:39][CH3:40])[CH:36]=[CH:35][C:4]=1[CH2:5][N:6]1[C:10]2[N:11]=[C:12]([C:15]3[C:23]4[C:18](=[N:19][CH:20]=[C:21]([F:24])[CH:22]=4)[N:17]([CH2:25][C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=4[F:32])[N:16]=3)[N:13]=[CH:14][C:9]=2[NH:8][S:7]1(=[O:34])=[O:33].[C:41](=O)([O-])[O-].[Cs+].[Cs+].IC>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:38]=[C:37]([O:39][CH3:40])[CH:36]=[CH:35][C:4]=1[CH2:5][N:6]1[C:10]2[N:11]=[C:12]([C:15]3[C:23]4[C:18](=[N:19][CH:20]=[C:21]([F:24])[CH:22]=4)[N:17]([CH2:25][C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=4[F:32])[N:16]=3)[N:13]=[CH:14][C:9]=2[N:8]([CH3:41])[S:7]1(=[O:34])=[O:33]

参加物

5

反応物 3

HCID 6328Methyl iodide2 回HCID 10796Cesium carbonateHCID 66635554HCID 66635554、化合物

生成物 1

HCID 66634917HCID 66634917、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

130 mg (approx. 0.115 mmol, 50% purity) of the compound from example 99A were initially charged in 5 ml of DMF, 44 mg (0.138 mmol) of cesium carbonate and 8.5 μl (0.138 mmol) of iodomethane were added and the mixture was stirred at RT overnight. Subsequently, another 14.3 μl (0.230 mmol) of iodomethane were added and the mixture was heated to 50° C. overnight. After cooling, the mixture was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient). This gave 30.9 mg (46% of theory) of the title compound.

後処理

  1. temperaturethe mixture was heated to 50° C. overnight
  2. temperatureAfter cooling
  3. customthe mixture was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient)

出典と根拠

ORDレコード
ord-ad5d4a5401fd4246bd0f4ec9c0a6c92b
出典データセット
uspto-grants-2015_08
特許番号
US09096592B2

反応ノート

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