Sodium Hydroxide → Trifluoroacetic acid

HRID 1987947ノート

反応式

HRID 1987947 の反応式
C1(S(O)(=O)=[O:8])C=CC=CC=1.[C:11]([NH:14][NH2:15])(=O)[CH3:12].[F:16][C:17]([F:45])([F:44])[C:18]([N:20]1[CH:25]2[CH2:26][CH2:27][CH:21]1[CH2:22][C:23](=[C:28]1[C:41]3[CH:40]=[CH:39][C:38]([C:42]#[N:43])=[CH:37][C:36]=3[O:35][C:34]3[C:29]1=[CH:30][CH:31]=[CH:32][CH:33]=3)[CH2:24]2)=[O:19].[OH-].[Na+]>CO>[CH3:12][C:11]1[NH:43][C:42]([C:38]2[CH:39]=[CH:40][C:41]3[C:28](=[C:23]4[CH2:22][CH:21]5[NH:20][CH:25]([CH2:26][CH2:27]5)[CH2:24]4)[C:29]4[C:34]([O:35][C:36]=3[CH:37]=2)=[CH:33][CH:32]=[CH:31][CH:30]=4)=[N:15][N:14]=1.[C:18]([OH:8])([C:17]([F:45])([F:44])[F:16])=[O:19]

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 577253399-[8-(2,2,2-Trifluoro-acetyl)-8-aza-bicyclo[3.2.1]oct-3-ylidene]-9H-xanthene-3-carbonitrileHCID 86636508Acetic hydrazide benzenesulfonic acid

生成物 2

HCID 6422Trifluoroacetic acidHCID 178433930HCID 178433930、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of compounds 11a (0.029 g, 0.125 mmol) and 5e (0.051g, 0.124 mmol) was exposed to microwave irradition (300 W) at 200° C. for 10 min. After cooling, MeOH (1 mL) and 1N NaOH (1 mL) were added to the reaction mixture and the mixture was stirred at rt for 30 min. The crude product was purified by reverse phase HPLC to yield compound 35 as a TFA salt. MS m/z (MH+) 371.0; 1H NMR (CH3OH-d4) δ 1.40 (d, 2H), 1.85 (m, 2H), 1.41 (s, 3H), 3.02 (m, 4H), 3.91 (m, 2H), 7.19 (m, 4H), 7.33 (d, 2H), 7.84 (d, 1H), 7.85 (s, 1H).

後処理

  1. temperatureAfter cooling
  2. customThe crude product was purified by reverse phase HPLC

出典と根拠

ORDレコード
ord-5844e01bb1154569be53d9dc0c6ea90d
出典データセット
uspto-grants-2009_06
特許番号
US07553850B2

反応ノート

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