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Hydrazine hydrate (1:1) → HCID 178514315, 화합물

HRID 1509312
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HRID 1509312 반응식
[Br:1][C:2]1[C:3]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:4][C:5]2[NH:10][C:9](=S)[CH2:8][O:7][C:6]=2[N:12]=1.O.[NH2:20][NH2:21]>O1CCCC1>[Br:1][C:2]1[C:3]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:4][C:5]2[NH:10]/[C:9](=[N:20]/[NH2:21])/[CH2:8][O:7][C:6]=2[N:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 866836666-bromo-7-phenyl-1H-pyrido[2,3-b][1,4]oxazine-2(3H)-thione

생성물 1

HCID 178514315HCID 178514315, 화합물수율 90.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In a 15 ml vial was 6-bromo-7-phenyl-1H-pyrido[2,3-b][1,4]oxazine-2(3H)-thione (100 mg, 0.311 mmol) and hydrazine monohydrate (0.049 ml, 1.557 mmol) in tetrahydrofuran (5 ml) to give a brown solution. The reaction mixture was stirred at room temperature for 1 hour. The reaction mixture was concentrated under reduced pressure and the crude residue was slurred in diethyl ether. The supernatant solvent was removed and the brown solid vas dried until constant weigh to afford the title compound (90 mg, 90%). It was used for the next step without further purification. LCMS (Method D): RT 0.770 min, M+1=321.

후처리

  1. customto give a brown solution
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customThe supernatant solvent was removed
  4. customthe brown solid vas dried

출처 및 근거

ORD 기록
ord-a954f6df6d8246caa17f62ca84978fe0
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09221838B2

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