Triphenylphosphine → 2-((7-Bromoquinolin-5-yloxy)methyl)nicotinamide

HRID 1402715ノート

反応式

HRID 1402715 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([OH:12])[C:5]2[CH:6]=[CH:7][CH:8]=[N:9][C:10]=2[CH:11]=1.O[CH2:14][C:15]1[N:23]=[CH:22][CH:21]=[CH:20][C:16]=1[C:17]([NH2:19])=[O:18].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(OC(N=NC(OC(C)(C)C)=O)=O)(C)(C)C>C(Cl)Cl.C1COCC1>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][CH:8]=[N:9]2)=[C:4]([O:12][CH2:14][C:15]2[N:23]=[CH:22][CH:21]=[CH:20][C:16]=2[C:17]([NH2:19])=[O:18])[CH:3]=1

参加物

7

反応物 4

HCID 11776TriphenylphosphineHCID 97268Di-tert-butyl azodicarboxylateHCID 139295182-(Hydroxymethyl)pyridine-3-carboxamideHCID 1362166197-Bromoquinolin-5-ol

生成物 1

HCID 712377752-((7-Bromoquinolin-5-yloxy)methyl)nicotinamide収率 45%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

100 mg 7-Bromo-quinolin-5-ol, 77.5 mg of 2-(hydroxymethyl)nicotinamide 3.7, 233.5 mg of triphenylphosphine and 205 mg of Di-tertbutyl-azodicarboxylate (DBAD) were dissolved in 2.5 mL of DCM and 7.5 mL of THF under Argon at room temperature. After 14 h the precipitate was collected and dried. The mother liquor was concentrated and the formed precipitate again collected to yield 72 mg Example 22.

後処理

  1. customat room temperature
  2. customAfter 14 h the precipitate was collected
  3. customdried
  4. concentrationThe mother liquor was concentrated
  5. customthe formed precipitate again collected

出典と根拠

ORDレコード
ord-bf44e5152414430c883c7962c9c0f1fd
出典データセット
uspto-grants-2014_12
特許番号
US08912173B2

反応ノート

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