Hydrochloric Acid → HCID 9840634、化合物

HRID 1354814ノート

反応式

HRID 1354814 の反応式
[OH-].[Na+].C([O:10][C:11](=[O:34])[C:12]1[CH:17]=[CH:16][C:15]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:14][C:13]=1[O:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)C1C=CC=CC=1.Cl>CO>[CH2:27]([O:26][C:13]1[CH:14]=[C:15]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:16]=[CH:17][C:12]=1[C:11]([OH:34])=[O:10])[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 15087000Phenylmethyl 2,4-bis(phenylmethoxy)benzoate

生成物 1

HCID 9840634HCID 9840634、化合物収率 38.92%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

NaOH (1 N) (150 mL) was added to compound 36 (4.3 g) in MeOH (50 mL). The reaction mixture was heated to 65° C. with stirring for 48 h. After the reaction mixture was cooled down to room temperature, 1.0 M HCl (200 mL) was added to neutralize the reaction mixture. The solvent was concentrated under reduced pressure. The residue was extracted with CHCl3 and H2O. The combined organic layer was dried over MgSO4. After the MgSO4 was filtered off, the solvent was removed under reduced pressure. The residue was purified by flash chromatography to give the compound 37 (1.3 g) as a solid with total yield of 38.92% for 2 steps. LC-MS (ESI): m/e=335.2 [M+1]+

後処理

  1. temperatureAfter the reaction mixture was cooled down to room temperature
  2. concentrationThe solvent was concentrated under reduced pressure
  3. extractionThe residue was extracted with CHCl3 and H2O
  4. dry with materialThe combined organic layer was dried over MgSO4
  5. filtrationAfter the MgSO4 was filtered off
  6. customthe solvent was removed under reduced pressure
  7. customThe residue was purified by flash chromatography

出典と根拠

ORDレコード
ord-385dc4a5f9c64d6d9acfe15963fdfeec
出典データセット
uspto-grants-2007_05
特許番号
US07223759B2

反応ノート

読み込み中…