Diazomethane → HCID 178497913、化合物

HRID 487064ノート

反応式

HRID 487064 の反応式
[N+](=[CH2:3])=[N-].[OH:4][C:5]1[N:13]=[C:12]([CH3:14])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=[O:8]>CCOCC.C1COCC1>[OH:4][C:5]1[N:13]=[C:12]([CH3:14])[CH:11]=[CH:10][C:6]=1[C:7]([O:9][CH3:3])=[O:8]

参加物

5

反応物 2

HCID 9550DiazomethaneHCID 178425908HCID 178425908、化合物

生成物 1

HCID 178497913HCID 178497913、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Excess diazomethane in ether was added portionwise over 15 mins to 9.58 g (~60 mmoles) of 2-hydroxy-6-methyl nicotinic acid in 900 mL of THF at 0°. After stirring 2 hours, excess diazomethane was removed in vacuo. The resulting white solid was filtered and washed with hexane and dried. This fluffy solid was the required methyl ester. The filtrate was concentrated. The resulting solid was redissolved in a minimum amount of THF and hexane was added until no further precipitation was observed. Solid was filtered and washed with hexane and dried to provide more of the desired compound.

後処理

  1. customexcess diazomethane was removed in vacuo
  2. filtrationThe resulting white solid was filtered
  3. washwashed with hexane
  4. customdried
  5. concentrationThe filtrate was concentrated
  6. dissolutionThe resulting solid was redissolved in a minimum amount of THF and hexane
  7. additionwas added until no further precipitation
  8. filtrationSolid was filtered
  9. washwashed with hexane
  10. customdried

出典と根拠

ORDレコード
ord-081eee156929442594546633c0e75235
出典データセット
uspto-grants-1994_03
特許番号
US05294610

反応ノート

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