Tetrahydrofuran → HCID 12901226、化合物

HRID 2051865ノート

反応式

HRID 2051865 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[C:10]([C:12]([OH:14])=O)[CH:11]=1)[NH:8][C:7](=[O:15])[CH2:6]2.O1CCCC1.[C:21]1([Li])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[C:10]([C:12](=[O:14])[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH:11]=1)[NH:8][C:7](=[O:15])[CH2:6]2

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 20378346HCID 20378346、化合物HCID 178506676HCID 178506676、化合物

生成物 1

HCID 12901226HCID 12901226、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A suspension of 1.0 g. (4.9 mmole) of 5-methoxy-7-carboxyindolin-2-one in 20 ml. of tetrahydrofuran was treated dropwise with 12 ml. of commercially prepared phenyllithium solution (2.3 molar ether: benzene; 0.28 moles). After stirring for two hours the reaction mixture was poured into water and extracted several times with ethyl ether and benzene. The combined extracts were washed with water, dried over sodium sulfate and concentrated using a rotary evaporator to a solid residue which on recrystallization from acetone-water gave 259 mg. (21%) of a yellow powder which melted at 154° C.

後処理

  1. additionA suspension of 1.0 g
  2. extractionextracted several times with ethyl ether and benzene
  3. washThe combined extracts were washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customa rotary evaporator to a solid residue which
  7. customon recrystallization from acetone-water
  8. customgave 259 mg

出典と根拠

ORDレコード
ord-5a32688342f44f6099cc80d1bc5c12e5
出典データセット
uspto-grants-1980_01
特許番号
US04182774

反応ノート

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