Formaldehyde → 5,6-Dihydroxy-N-methylisoindoline hydrobromide

HRID 704459노트

반응식

HRID 704459 반응식
[BrH:1].[OH:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[OH:12])[CH2:8][NH:7][CH2:6]2.[CH:13]([O-])=O.[Na+].C=O>C(O)=O>[BrH:1].[OH:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[OH:12])[CH2:8][N:7]([CH3:13])[CH2:6]2

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 2723810Sodium FormateHCID 200743492,3-dihydro-1H-isoindole-5,6-diol hydrobromide

생성물 1

HCID 140984225,6-Dihydroxy-N-methylisoindoline hydrobromide수율 72.3%

시약·촉매·용매 1

HCID 284Formic Acid용매

반응 조건

온도
80 °C

실험 절차

15.39 g (66 mmol) of 5,6-dihydroxyisoindoline hydrobromide and 4.48 g (66 mmol) of sodium formate were dissolved in 100 ml of a 50% formic acid aqueous solution, and then 5.17 ml (70 mmol) of 37% formalin was added thereto. The mixture was heated at 80° C. for 4 hours. Then, the reaction solvent was distilled off under reduced pressure, and 200 ml of 23% hydrobromic acid was added to the residue. The mixture was subjected to active carbon treatment. The filtrate was again evaporated under reduced pressure to dryness, and the crystalline residue was recrystallized from water to obtain 11.74 g (yield: 72.3%) of the above identified compound.

후처리

  1. distillationThen, the reaction solvent was distilled off under reduced pressure, and 200 ml of 23% hydrobromic acid
  2. additionwas added to the residue
  3. customThe filtrate was again evaporated under reduced pressure to dryness
  4. customthe crystalline residue was recrystallized from water
  5. customto obtain 11.74 g (yield: 72.3%) of the

출처 및 근거

ORD 기록
ord-8103f4452ed944e8971517097f65c53b
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04987235

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