Water → HCID 10303760、化合物

HRID 858327

反応式

HRID 858327 の反応式
[CH2:1]([C:5]1[O:6][C:7]2[CH:22]=[CH:21][C:20]([CH2:23][OH:24])=[CH:19][C:8]=2[C:9]=1[C:10](=[O:18])[C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][CH:12]=1)[CH2:2][CH2:3][CH3:4].Cl[CH2:26][CH2:27][CH2:28][N:29]([CH2:34][CH2:35][CH2:36][CH3:37])[CH2:30][CH2:31][CH2:32][CH3:33].[C:38](=[O:41])([O-:40])[O-].[K+].[K+].[OH2:44]>C(C(C)=O)C>[C:23]([OH:24])(=[O:44])[C:38]([OH:40])=[O:41].[CH2:1]([C:5]1[O:6][C:7]2[CH:22]=[CH:21][C:20]([CH2:23][OH:24])=[CH:19][C:8]=2[C:9]=1[C:10](=[O:18])[C:11]1[CH:12]=[CH:13][C:14]([O:17][CH2:26][CH2:27][CH2:28][N:29]([CH2:34][CH2:35][CH2:36][CH3:37])[CH2:30][CH2:31][CH2:32][CH3:33])=[CH:15][CH:16]=1)[CH2:2][CH2:3][CH3:4]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 96084N-(3-Chloropropyl)dibutylamineHCID 69360765HCID 69360765、化合物

生成物 1

HCID 10303760HCID 10303760、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

1.68 g of 2-butyl-3-(4-hydroxybenzoyl)-5-hydroxymethyl-1-benzofuran, 1.18 g of 1-chloro-3-(dibutylamino)propane and 0.960 g of potassium carbonate are dissolved in 70 ml of methyl ethyl ketone. The mixture is brought to reflux for 6 hours, water is added and separation is carried out by settling. Extraction with ethyl acetate and washing with a saturated sodium chloride solution are carried out. Purification is subsequently carried out by chromatography on silica (eluent: 95/5 dichloromethane/methanol), which gives the desired compound in the free base form.

後処理

  1. temperatureto reflux for 6 hours
  2. customseparation
  3. extractionExtraction with ethyl acetate
  4. washwashing with a saturated sodium chloride solution
  5. customPurification

出典と根拠

ORDレコード
ord-d20917c659e24f4b831aac7e156c6639
出典データセット
uspto-grants-2006_12
特許番号
US07148240B2

関連ノート

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