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Stannous chloride dihydrate → HCID 59427335、化合物

HRID 1013704
ノート
印刷プレビュー

反応式

HRID 1013704 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 61436Stannous chloride dihydrate2 回HCID 59427359HCID 59427359、化合物

生成物 1

HCID 59427335HCID 59427335、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-362611cf3b654dff811fffa516f2894f
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07981891B2

反応ノート

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