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HCID 58537898, 화합물 → HCID 58537924, 화합물

HRID 570098
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HRID 570098 반응식
C([O:8][C:9]1[C:13]2([CH2:18][CH2:17][N:16]([O:19][CH3:20])[CH2:15][CH2:14]2)[N:12]([CH2:21][CH:22]2[CH2:24][CH2:23]2)[C:11](=[O:25])[C:10]=1[C:26]1[C:31]([CH3:32])=[CH:30][C:29]([CH3:33])=[CH:28][C:27]=1[CH3:34])C1C=CC=CC=1>CO.[Pd]>[CH:22]1([CH2:21][N:12]2[C:13]3([CH2:14][CH2:15][N:16]([O:19][CH3:20])[CH2:17][CH2:18]3)[C:9]([OH:8])=[C:10]([C:26]3[C:27]([CH3:34])=[CH:28][C:29]([CH3:33])=[CH:30][C:31]=3[CH3:32])[C:11]2=[O:25])[CH2:24][CH2:23]1
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참가 물질

4

반응물 1

HCID 58537898HCID 58537898, 화합물

생성물 1

HCID 58537924HCID 58537924, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

Debenzylation was conducted using an H-Cube® continuous-flow hydrogenator: 4-benzyloxy-1-cyclopropylmethyl-8-methoxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-one (546 mg, 1.34 mmol) was dissolved in methanol (47 ml) and this substrate solution (0.029 M) pumped twice through a 5% Pd/C filled cartridge at a flow-rate of 1 mL/min, a temperature of 35° C. and a pressure of 2-3 bars. The collected product solution was concentrated, and the residue purified by chromatography on silica gel (ethyl acetate/heptane 1:1). Yield: 215 mg of 1-cyclopropylmethyl-4-hydroxy-8-methoxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-one (title compound P2.8) as a white solid, mp 223-225° C.

후처리

  1. customa temperature of 35° C.
  2. concentrationThe collected product solution was concentrated
  3. customthe residue purified by chromatography on silica gel (ethyl acetate/heptane 1:1)

출처 및 근거

ORD 기록
ord-6e59bf793ede439baead50cdd65e7e53
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09023760B2

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