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

HRID 2105045노트

반응식

HRID 2105045 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-5a2bd46f56a440dfb0392e5f85ce7480
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576098B2

반응 노트

불러오는 중…