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Stannous chloride dihydrate → HCID 59427335, 화합물

HRID 1013704
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HRID 1013704 반응식
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([CH:13]([C:15]3[CH:20]=[CH:19][C:18]([N+:21]([O-])=O)=[CH:17][CH:16]=3)O)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.O.O.[Sn](Cl)Cl>CO>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([CH2:13][C:15]3[CH:16]=[CH:17][C:18]([NH2:21])=[CH:19][CH:20]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 61436Stannous chloride dihydrate2회HCID 59427359HCID 59427359, 화합물

생성물 1

HCID 59427335HCID 59427335, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

A mixture of (7-methoxyquinolin-4-yl)(4-nitrophenyl)methanol (0.187 g, 0.603 mmol) and tin(II) chloride dihydrate (0.823 g, 3.62 mmol) in MeOH (10 mL) was heated to 60° C. After 1 hr an additional 5 eq of tin(II) chloride dihydrate was added. After 3 hrs, the mixture was concentrated in vacuo and diluted with EtOAc and water. Saturated NaHCO3 was added until the aqueous layer was basic. The resulting suspension was filtered and the solids washed with EtOAc. The organic fraction was washed with water, brine, and dried with Na2SO4. After concentrating in vacuo, the crude, yellow solid, 4-((7-methoxyquinolin-4-yl)methyl)benzenamine was advanced without further purification. MS found: M+H+=265.1.

후처리

  1. concentrationthe mixture was concentrated in vacuo
  2. additiondiluted with EtOAc and water
  3. additionSaturated NaHCO3 was added until the aqueous layer
  4. filtrationThe resulting suspension was filtered
  5. washthe solids washed with EtOAc
  6. washThe organic fraction was washed with water, brine
  7. dry with materialdried with Na2SO4
  8. concentrationAfter concentrating in vacuo
  9. customthe crude, yellow solid, 4-((7-methoxyquinolin-4-yl)methyl)benzenamine was advanced without further purification

출처 및 근거

ORD 기록
ord-362611cf3b654dff811fffa516f2894f
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981891B2

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