Hydrochloric Acid → 4-[3-[6-(3-Benzylcarbamoyl-5-iodo-phenoxy)-hexyl]-2-(2-carboxy-ethyl)-phenoxy]-butyric Acid

HRID 1670072ノート

反応式

HRID 1670072 の反応式
C([O:3][C:4](=[O:46])[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:27]=[C:26]([I:28])[CH:25]=[C:24]([C:29](=[O:38])[NH:30][CH2:31][C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)[CH:23]=2)[C:10]=1[CH2:39][CH2:40][C:41]([O:43]CC)=[O:42])C.[OH-].[Na+].Cl>C1COCC1>[CH2:31]([NH:30][C:29]([C:24]1[CH:23]=[C:22]([CH:27]=[C:26]([I:28])[CH:25]=1)[O:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:11]1[C:10]([CH2:39][CH2:40][C:41]([OH:43])=[O:42])=[C:9]([CH:14]=[CH:13][CH:12]=1)[O:8][CH2:7][CH2:6][CH2:5][C:4]([OH:46])=[O:3])=[O:38])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 673378574-[3-[6-(3-Benzylcarbamoyl-5-iodo-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric Acid Ethyl Ester

生成物 1

HCID 673379344-[3-[6-(3-Benzylcarbamoyl-5-iodo-phenoxy)-hexyl]-2-(2-carboxy-ethyl)-phenoxy]-butyric Acid収率 100.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
55 °C

実験手順

4-[3-[6-(3-Benzylcarbamoyl-5-iodo-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (8.7 g) was dissolved in THF (30 mL) and 2 M NaOH was added (30 mL). The resulting heterogeneous mixture was stirred vigorously at 55° C. for 4 h. Then it was acidified with 3 N HCl and extracted into diethyl ether. Etherate extract was washed with brine and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to produce 8.1 g (100% yield) of colorless oil which solidified upon standing.

後処理

  1. extractionextracted into diethyl ether
  2. extractionEtherate extract
  3. washwas washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-768ba9ba868c480498bb55fcb16a6b24
出典データセット
uspto-grants-2011_08
特許番号
US07989454B2

反応ノート

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