2-Butanamine, 2-methyl- → HCID 22922542, 화합물

HRID 2258545

반응식

HRID 2258545 반응식
[C:1]([NH:5][C:6]([C:8]1[CH:33]=[CH:32][C:11]([CH2:12][N:13]2[C:17]3[CH:18]=[CH:19][C:20]([O:22][CH2:23][CH3:24])=[CH:21][C:16]=3[N:15]([CH:25]3[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]3)[C:14]2=[O:31])=[C:10]([O:34][CH3:35])[CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=C[C:46]=2N=N1.CCN(C(C)C)C(C)C.C(N)(CC)(C)C>C(Cl)Cl>[CH:25]1([N:15]2[C:16]3[CH:21]=[C:20]([O:22][CH2:23][CH3:24])[CH:19]=[CH:18][C:17]=3[N:13]([CH2:12][C:11]3[CH:32]=[CH:33][C:8]([C:6](=[O:7])[NH:5][C:1]([CH3:4])([CH3:2])[CH2:3][CH3:46])=[CH:9][C:10]=3[O:34][CH3:35])[C:14]2=[O:31])[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1

참가 물질

6

반응물 4

HCID 689862-Butanamine, 2-methyl-HCID 81531DiisopropylethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 229224911-[4-(N-tert-Butylcarbamoyl)-2-methoxybenzyl]-3-cyclohexyl-5-ethoxy-1,3-dihydro-2H-benzimidazol-2-one

생성물 1

HCID 22922542HCID 22922542, 화합물수율 36.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.9 g of the compound obtained in Example 15 Step B, 0.9 g of BOP and 1 ml of DIPEA in 20 ml of DCM is added 1 g of tert-amylamine, and the mixture is left stirring for 3 hours at RT. The reaction mixture is washed with 1N HCl solution, with 1N NaOH solution and dried over Na2SO4, and the solvent is evaporated off under vacuum. The residue is chromatographed on silica, eluting with DCM. 0.34 g of the expected product is obtained, mp=164° C.

후처리

  1. waitthe mixture is left
  2. washThe reaction mixture is washed with 1N HCl solution, with 1N NaOH solution
  3. dry with materialdried over Na2SO4
  4. customthe solvent is evaporated off under vacuum
  5. customThe residue is chromatographed on silica
  6. washeluting with DCM

출처 및 근거

ORD 기록
ord-f55ae4b4c20a4304814809370b70318a
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05661169

연결된 노트

불러오는 중…