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Benzyl Bromide → HCID 86606713, 화합물

HRID 1012849
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HRID 1012849 반응식
[CH2:1]([Br:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl.[N:16]12[CH2:23][CH2:22][CH:19]([CH2:20][CH2:21]1)[C@@H:18]([NH:24][C:25]([C:27]1[O:28][C:29]3[C:35]([C:36]4[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=4[O:42][CH3:43])=[CH:34][CH:33]=[CH:32][C:30]=3[CH:31]=1)=[O:26])[CH2:17]2>CN(C=O)C>[Br-:8].[CH2:1]([N+:16]12[CH2:21][CH2:20][CH:19]([CH2:22][CH2:23]1)[C@@H:18]([NH:24][C:25]([C:27]1[O:28][C:29]3[C:35]([C:36]4[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=4[O:42][CH3:43])=[CH:34][CH:33]=[CH:32][C:30]=3[CH:31]=1)=[O:26])[CH2:17]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 67312922HCID 67312922, 화합물

생성물 1

HCID 86606713HCID 86606713, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

288 μl (2.42 mmol) of benzyl bromide and 502 mg (3.63 mmol) of potassium carbonate are added to a solution of 500 mg (1.21 mmol) of N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-7-(2-methoxyphenyl)-1-benzofuran-2-carboxamide hydrochloride (Example 102) in 12.5 ml of DMF. After 20 h at 50° C., the reaction mixture is purified by preparative HPLC. The product fractions are concentrated and, after addition of 50% strength hydrobromic acid, again concentrated and dried under high vacuum. Recrystallization from cyclohexane/acetone affords 537 mg (77% of theory) of the title compound.

후처리

  1. customthe reaction mixture is purified by preparative HPLC
  2. concentrationThe product fractions are concentrated
  3. additionafter addition of 50% strength hydrobromic acid
  4. concentrationagain concentrated
  5. customdried under high vacuum
  6. customRecrystallization from cyclohexane/acetone

출처 및 근거

ORD 기록
ord-1b9ab4c5332e4d87b5d175b4604df591
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07977485B2

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