trans-1-Boc-4-aminomethyl-3-hydroxypiperidine → HCID 11015727, 화합물

HRID 353342

반응식

HRID 353342 반응식
[NH2:1][CH2:2][C@@H:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][C@H:4]1[OH:16].[NH2:17][C:18]1[C:30]([Cl:31])=[CH:29][C:21]([C:22](N2C=CN=C2)=[O:23])=[C:20]([O:32][CH3:33])[C:19]=1[O:34][CH3:35]>C(#N)C>[NH2:17][C:18]1[C:30]([Cl:31])=[CH:29][C:21]([C:22]([NH:1][CH2:2][C@@H:3]2[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:13])([CH3:15])[CH3:14])=[O:10])[CH2:5][C@H:4]2[OH:16])=[O:23])=[C:20]([O:32][CH3:33])[C:19]=1[O:34][CH3:35]

참가 물질

4

반응물 2

HCID 11075229trans-1-Boc-4-aminomethyl-3-hydroxypiperidineHCID 88040818HCID 88040818, 화합물

생성물 1

HCID 11015727HCID 11015727, 화합물수율 80%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of intermediate (1-e) (0.087 mol) and intermediate (3-a) (0.087 mol) in acetonitrile (600 ml) was stirred and refluxed for 90 min. The reaction mixture was cooled, and the solvent was evaporated. The residue was partitioned between DCM and water. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was suspended in DIPE with a drop of ACN, filtered off and dried (vacuum, 40° C.), yielding 30.3 g (80%) of (±)-1,1-dimethylethyl trans-4-[[(4-amino-5-chloro-2,3-dimethoxybenzoyl)amino]methyl]-3-hydroxy-1-piperidinecarboxylate (interm. 4).

후처리

  1. temperaturerefluxed for 90 min
  2. temperatureThe reaction mixture was cooled
  3. customthe solvent was evaporated
  4. customThe residue was partitioned between DCM and water
  5. customThe organic layer was separated
  6. customdried
  7. filtrationfiltered
  8. customthe solvent was evaporated
  9. filtrationfiltered off
  10. customdried (vacuum, 40° C.)

출처 및 근거

ORD 기록
ord-f649c2ede5634f988e45339bcfac2953
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06750349B2

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