Tetrahydrofuran → HCID 12901226, 화합물

HRID 1704319노트

반응식

HRID 1704319 반응식
[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

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 20378346HCID 20378346, 화합물HCID 178506676HCID 178506676, 화합물

생성물 1

HCID 12901226HCID 12901226, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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 2 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.

후처리

  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

출처 및 근거

ORD 기록
ord-b11ea9c4aeb9422dae9dc41bf3a8455e
출처 데이터셋
uspto-grants-1978_11
특허 번호
US04126635

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