Oxalic Acid → 1-{2-[2-(1-Benzothiophen-6-yl)ethoxy]ethyl}-3-pyrrolidinol oxalate

HRID 7443

反応式

HRID 7443 の反応式
[S:1]1[C:5]2[CH:6]=[C:7]([CH2:10][CH2:11][O:12][CH2:13][CH2:14][N:15]3[CH2:19][CH2:18][CH:17]([OH:20])[CH2:16]3)[CH:8]=[CH:9][C:4]=2[CH:3]=[CH:2]1.[C:21]([OH:26])(=[O:25])[C:22]([OH:24])=[O:23]>C(OCC)(=O)C>[C:21]([OH:26])(=[O:25])[C:22]([OH:24])=[O:23].[S:1]1[C:5]2[CH:6]=[C:7]([CH2:10][CH2:11][O:12][CH2:13][CH2:14][N:15]3[CH2:19][CH2:18][CH:17]([OH:20])[CH2:16]3)[CH:8]=[CH:9][C:4]=2[CH:3]=[CH:2]1

参加物

4

反応物 2

HCID 971Oxalic AcidHCID 219900201-{2-[2-(1-Benzothiophen-6-yl)ethoxy]ethyl}-3-pyrrolidinol

生成物 1

HCID 219901241-{2-[2-(1-Benzothiophen-6-yl)ethoxy]ethyl}-3-pyrrolidinol oxalate収率 66.8%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

In 2.0 mL of ethyl acetate was dissolved 0.48 g of 1-{2-[2-(1-benzothiophen-6-yl)ethoxy]ethyl}-3-pyrrolidinol, and to the solution was added a solution of 0.15 g of oxalic acid in 2.8 mL of ethyl acetate. The resulting mixture was stirred at room temperature for 1 hour and then at 5° C. for 1 hour. The crystals precipitated were collected by filtration, washed with ethyl acetate and then dried to obtain 0.42 g of 1-{2-[2-(1-benzothiophen-6-yl)ethoxy]ethyl}-3-pyrrolidinol oxalate as colorless crystals.

後処理

  1. waitat 5° C. for 1 hour
  2. customThe crystals precipitated
  3. filtrationwere collected by filtration
  4. washwashed with ethyl acetate
  5. customdried

出典と根拠

ORDレコード
ord-5c19260c8f004085a305aaa6379d532c
出典データセット
uspto-grants-2006_08
特許番号
US07087594B2

関連ノート

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