Carbon tetrabromide → HCID 68514522, 화합물

HRID 1717391노트

반응식

HRID 1717391 반응식
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]

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 57665111HCID 57665111, 화합물

생성물 1

HCID 68514522HCID 68514522, 화합물수율 50%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-6bc6c0c2213d4403a1df2e92fc6bd5f3
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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