Water → 3,5-dibromo-1-trityl-1H-1,2,4-triazole

HRID 2105045ノート

反応式

HRID 2105045 の反応式
[C:1](Cl)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Br:21][C:22]1[N:26]=[C:25]([Br:27])[NH:24][N:23]=1.C(N(CC)CC)C.O>CN(C=O)C>[Br:21][C:22]1[N:26]=[C:25]([Br:27])[N:24]([C:1]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[N:23]=1

参加物

6

反応物 4

HCID 962WaterHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 819043,5-Dibromo-4H-1,2,4-triazole

生成物 1

HCID 578040363,5-dibromo-1-trityl-1H-1,2,4-triazole収率 98.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Trityl chloride (6.8 g, 24 mmol) was added to a solution of 3,5-dibromo-1H-1,2,4-triazole (5 g, 22 mmol) and triethylamine (3.4 mL, 24.2 mmol) in DMF (100 mL) and stirred 16 h. The mixture was poured into rapidly stirred water (300 mL). The white precipitate was collected, washed with hexanes and dried on high vacuum to yield 10.2 g of Intermediate 359.1 as a white solid. 1H NMR (400 MHz, CDCl3) δ ppm 7.09-7.17 (m, 6H) 7.28-7.35 (m, 9H).

後処理

  1. customThe white precipitate was collected
  2. washwashed with hexanes
  3. customdried on high vacuum

出典と根拠

ORDレコード
ord-5a2bd46f56a440dfb0392e5f85ce7480
出典データセット
uspto-grants-2009_08
特許番号
US07576098B2

反応ノート

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