Triethylsilane → HCID 66635174、化合物

HRID 510144ノート

反応式

HRID 510144 の反応式
COC1C=C(OC)C=CC=1C[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]([CH3:33])[S:7]1(=[O:35])=[O:34].C([SiH](CC)CC)C>FC(F)(F)C(O)=O>[F:24][C:21]1[CH:22]=[C:23]2[C:15]([C:12]3[N:13]=[CH:14][C:9]4[N:8]([CH3:33])[S:7](=[O:34])(=[O:35])[NH:6][C:10]=4[N:11]=3)=[N:16][N:17]([CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[F:32])[C:18]2=[N:19][CH:20]=1

参加物

4

反応物 2

HCID 12052TriethylsilaneHCID 66634917HCID 66634917、化合物

生成物 1

HCID 66635174HCID 66635174、化合物

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

28 mg (0.050 mmol) of the compound from example 100A were dissolved in 1.5 ml of trifluoroacetic acid and then admixed with 79 μl (0.495 mmol) of triethylsilane, and the mixture was heated to reflux overnight. This was followed by concentration to dryness. After purification by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient), this gave 10.4 mg (48% of theory) of the title compound.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux overnight
  3. concentrationThis was followed by concentration to dryness
  4. customAfter purification by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient)

出典と根拠

ORDレコード
ord-11dc3467c9e14bc6bb633252a589f161
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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