Piperidine → (S)-tert-Butyl 2-(2-amino-3-(4-hydroxyphenyl)propanamido)acetate

HRID 1755481노트

반응식

HRID 1755481 반응식
C1C2C(COC([NH:18][C@@H:19]([CH2:31][C:32]3[CH:37]=[CH:36][C:35]([OH:38])=[CH:34][CH:33]=3)[C:20]([NH:22][CH2:23][C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])=[O:21])=O)C3C(=CC=CC=3)C=2C=CC=1.N1CCCCC1>CN(C=O)C>[NH2:18][C@@H:19]([CH2:31][C:32]1[CH:37]=[CH:36][C:35]([OH:38])=[CH:34][CH:33]=1)[C:20]([NH:22][CH2:23][C:24]([O:26][C:27]([CH3:30])([CH3:28])[CH3:29])=[O:25])=[O:21]

참가 물질

4

반응물 2

HCID 8082PiperidineHCID 86700124(S)-tert-Butyl 2-(2-(((9H-fluoren-9-yl)methoxy)carbonylamino)-3-(4-hydroxyphenyl)propanamido)acetate

생성물 1

HCID 86700125(S)-tert-Butyl 2-(2-amino-3-(4-hydroxyphenyl)propanamido)acetate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution material from Example 97 (4.7 g, 9.10 mmol) in anhydrous DMF (30 mL) is added piperidine (15 mL, 152 mmol). The resulting solution is stirred at room temp for 45 rain and the solvent is removed in vacuo. The resulting residue was redissolved in 1,4-dioxane (50 mL), the solvent was removed in vacuo again and the resulting solid was dried under high vacuum for 18 h to give the title compound as a white solid in quantitative yield that contains 1 equivalent of 1-((9H-fluoren-9-yl)methyl)piperidine as a side product. LC/MS (Condition A): ret. T=2.30 rain, (M+H)+ 295.

후처리

  1. customthe solvent is removed in vacuo
  2. dissolutionThe resulting residue was redissolved in 1,4-dioxane (50 mL)
  3. customthe solvent was removed in vacuo again
  4. customthe resulting solid was dried under high vacuum for 18 h

출처 및 근거

ORD 기록
ord-501da06283154387a78b5e9bdd6f2590
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169295B2

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