Acetonitrile → HCID 23135106、化合物

HRID 254277

反応式

HRID 254277 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][NH:6][C:7]([CH:9]1[CH:18]=[CH:17][C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH2:10]1)=[O:8].[OH:19][C:20]1[CH:21]=[C:22](N2CCNCC2)[CH:23]=[CH:24][CH:25]=1.C([N:34]([CH2:37][CH3:38])[CH2:35][CH3:36])C.CC#[N:41]>>[OH:19][C:20]1[CH:21]=[C:22]([CH:35]2[CH2:36][NH:41][CH2:38][CH2:37][N:34]2[CH2:2][CH2:3][CH2:4][CH2:5][NH:6][C:7]([C:9]2[CH2:18][CH2:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH:10]=2)=[O:8])[CH:23]=[CH:24][CH:25]=1

参加物

5

反応物 4

HCID 6342AcetonitrileHCID 8471TriethylamineHCID 27365971-(3-Hydroxyphenyl)piperazineHCID 66852491HCID 66852491、化合物

生成物 1

HCID 23135106HCID 23135106、化合物収率 54%

実験手順

A mixture of the bromo adduct E1 (100 mg, 0.32 mmol), of commercial 3-hydroxyphenyl piperazine (57 mg, 0.32 mmol) and triethylamine (0.07 mL, 0.5 mmol) in CH3CN are reluxed during 16 h. The solvent is evaporated and the residue is taken up in CH2Cl2 (15 mL), washed with brine, dried and concentrated. The residue is purified by chromatography eluting with AcOEt:MeOH (9/1) to yield the titled adduct (mp 152° C., 70 mg, 54%)

後処理

  1. customThe solvent is evaporated
  2. washwashed with brine
  3. customdried
  4. concentrationconcentrated
  5. customThe residue is purified by chromatography
  6. washeluting with AcOEt

出典と根拠

ORDレコード
ord-d5c811394752484d9f35c8383a6030e7
出典データセット
uspto-grants-2011_01
特許番号
US07875617B2

関連ノート

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