Carbon tetrabromide → HCID 68514522、化合物

HRID 1717391ノート

反応式

HRID 1717391 の反応式
O[CH2:2][CH2:3][CH2:4][C:5]1[N:9]([C:10]2[CH:15]=[CH:14][C:13]([C:16]([NH:18][CH2:19][C:20]([F:23])([F:22])[F:21])=[O:17])=[CH:12][CH:11]=2)[N:8]=[N:7][C:6]=1[C:24]([NH2:26])=[O:25].C1(P([C:40]2[CH:45]=[CH:44]C=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Br:46]C(Br)(Br)Br>ClCCl>[Br:46][CH2:2][CH2:3][CH2:4][C:5]1[N:9]([C:10]2[CH:11]=[CH:12][C:13]([C:16]([NH:18][CH2:19][C:20]([F:22])([F:21])[F:23])=[O:17])=[CH:14][CH:15]=2)[N:8]=[N:7][C:6]=1[C:24]([NH:26][CH:44]1[CH2:45][CH2:40]1)=[O:25]

参加物

5

反応物 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 57665111HCID 57665111、化合物

生成物 1

HCID 68514522HCID 68514522、化合物収率 50%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-(3-hydroxypropyl)-1-(4-{[(2,2,2-trifluoroethyl)amino]carbonyl}phenyl)-1H-1,2,3-triazole-4-carboxamide (381 mg, 0.93 mmol) obtained in Example 398 and triphenylphosphine (365 mg) in dichloromethane (12 ml) was added tetrabromomethane (460 mg), and the mixture was stirred at room temperature for 15 hr. The reaction mixture was concentrated under reduced pressure, and the obtained residue was purified by silica gel column (hexane/ethyl acetate=20/1 to 2/5) to give the title compound as a colorless solid (219 mg, 50%).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe obtained residue was purified by silica gel column (hexane/ethyl acetate=20/1 to 2/5)

出典と根拠

ORDレコード
ord-6bc6c0c2213d4403a1df2e92fc6bd5f3
出典データセット
uspto-grants-2010_09
特許番号
US07803822B2

反応ノート

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