Sulfuric Acid → HCID 86723684, 화합물

HRID 577446노트

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HRID 577446 반응식
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=O)=[CH:4][C:3]=1[O:11][CH3:12].CN(C(O[N:21]1N=N[C:23]2C=CC=N[C:22]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.COC(OC)CN.OS(O)(=O)=O.[OH-].[Na+]>S1(CCCC1)(=O)=O>[F:1][C:2]1[CH:10]=[C:9]2[C:5](=[CH:4][C:3]=1[O:11][CH3:12])[C:6](=[O:8])[NH:21][CH:22]=[CH:23]2

참가 물질

7

반응물 5

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 89728Aminoacetaldehyde dimethyl acetalHCID 5984364-Fluoro-3-methoxybenzoic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

생성물 1

HCID 86723684HCID 86723684, 화합물수율 89.4%

시약·촉매·용매 1

HCID 31347Sulfolane용매

실험 절차

A solution of 4-fluoro-3-methoxybenzoic acid (1.30 g, 7.64 mmol) and TEA (1.25 mL, 8.97 mmol) in sulfolane (6.0 mL) was treated with HATU (3.25 g, 8.55 mmol). After 10 minutes, aminoacetaldehyde dimethylacetal (0.925 mL, 8.58 mmol) was added. The reaction mixture was stirred at room temperature for 30 minutes. The reaction mixture was then treated with conc. H2SO4 (15 mL) and stirred at 60° C. for 2 days. The reaction mixture was poured over ice and brought to pH˜4 with 10M NaOH (˜55 mL). The precipitate was collected by filtration, washed with water, and dried under vacuum to give 6-fluoro-7-methoxyisoquinolin-1(2H)-one (Cpd L, 1.32 g, 89%) as a white powder.

후처리

  1. stirringstirred at 60° C. for 2 days
  2. additionThe reaction mixture was poured over ice
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-fdb5560e7aab40d19ff9338fd477821a
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040515B2

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