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hydroxylamine-O-sulfonic acid → HCID 13669915, 화합물

HRID 256316
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HRID 256316 반응식
[CH2:1]([C:3]1[C:4]([O:15][CH3:16])=[N:5][C:6]2[N:7]([CH:10]=[C:11]([CH:13]=O)[N:12]=2)[C:8]=1[CH3:9])[CH3:2].[NH2:17]OS(O)(=O)=O>O>[CH2:1]([C:3]1[C:4]([O:15][CH3:16])=[N:5][C:6]2[N:7]([CH:10]=[C:11]([C:13]#[N:17])[N:12]=2)[C:8]=1[CH3:9])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 76284hydroxylamine-O-sulfonic acidHCID 13304948HCID 13304948, 화합물

생성물 1

HCID 13669915HCID 13669915, 화합물수율 83%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a rapidly stirred suspension of 19.84 g of 6-ethyl-7-methoxy-5-methylimidazo[1,2-a]pyrimidine-2-carboxaldehyde in 300 ml of water at room temperature was added all at once a solution of 13.30 g of hydroxylamine-o-sulfonic acid in 250 ml of water. After 40 minutes when the intermediate had precipitated, 8 g of solid sodium hydroxide were added and the intermediate dissolved. After 1 hour when the product had precipitated, the mixture was filtered and the solid was washed with water, dried, then crystallized from ethyl acetate to obtain 16.18 g of 6-ethyl-7-methoxy-5-methylimidazo [1,2-a]pyrimidine-2-carbonitrile (83% yield) as a pale yellow solid melting at 166°-168° C.

후처리

  1. customAfter 40 minutes when the intermediate had precipitated
  2. addition8 g of solid sodium hydroxide were added
  3. dissolutionthe intermediate dissolved
  4. customAfter 1 hour when the product had precipitated
  5. filtrationthe mixture was filtered
  6. washthe solid was washed with water
  7. customdried
  8. customcrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-61c774323e444bc5bf8cd0183172ac0a
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04703049

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