Water → HCID 59639634, 화합물

HRID 2250097노트

반응식

HRID 2250097 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]1[C:14]2[N:15]=[C:16]([NH:27][CH2:28][C:29]([NH:31][CH2:32][CH2:33][O:34]C)=[O:30])[N:17]=[C:18]([C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:20]=3[CH3:26])[C:13]=2[CH:12]=[CH:11][C:10]1=[O:36].B(Br)(Br)Br.O>ClCCl>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]1[C:14]2[N:15]=[C:16]([NH:27][CH2:28][C:29]([NH:31][CH2:32][CH2:33][OH:34])=[O:30])[N:17]=[C:18]([C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:20]=3[CH3:26])[C:13]=2[CH:12]=[CH:11][C:10]1=[O:36]

참가 물질

5

반응물 3

HCID 962WaterHCID 25134Boron tribromideHCID 59639571HCID 59639571, 화합물

생성물 1

HCID 59639634HCID 59639634, 화합물수율 62.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a soln of the product of Example 205 (50 mg, 0.1 mmol), in dichloromethane (2 mL) was added 1 M boron tribromide in dichloromethane (0.5 mL, 0.5 mmol). The mixture was stirred at 23° for 2 h, H2O was added, extracted with EtOAc. The organic layer was dried (Na2SO4) and concentrated to give the crude material. Recrystallization from dichloromethane and hexane afforded the title product (30 mg, 62%). LC-MS: 484.2 (MH+, m/z), 1.59 (Rt, min).

후처리

  1. extractionextracted with EtOAc
  2. dry with materialThe organic layer was dried (Na2SO4)
  3. concentrationconcentrated
  4. customto give the crude material
  5. customRecrystallization from dichloromethane and hexane

출처 및 근거

ORD 기록
ord-8c658292272b459b90230b682a58863b
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07314934B2

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