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Triphenylphosphine → 9-benzyloxy-6-[1-(4-chlorophenyl)-cyclopentylmethyl]-2-cyclopropyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione

HRID 2169363
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HRID 2169363 반응식
[CH:1]1([N:4]([CH2:35][CH2:36]O)[C:5]([C:7]2[C:12]([O:13][CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[C:11]([OH:21])[N:10]=[C:9]([CH2:22][C:23]3([C:28]4[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=4)[CH2:27][CH2:26][CH2:25][CH2:24]3)[N:8]=2)=[O:6])[CH2:3][CH2:2]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>ClCCl>[CH2:14]([O:13][C:12]1[C:11](=[O:21])[N:10]=[C:9]([CH2:22][C:23]2([C:28]3[CH:29]=[CH:30][C:31]([Cl:34])=[CH:32][CH:33]=3)[CH2:27][CH2:26][CH2:25][CH2:24]2)[N:8]2[CH2:36][CH2:35][N:4]([CH:1]3[CH2:2][CH2:3]3)[C:5](=[O:6])[C:7]=12)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 178519969HCID 178519969, 화합물

생성물 1

HCID 867259949-benzyloxy-6-[1-(4-chlorophenyl)-cyclopentylmethyl]-2-cyclopropyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione수율 151.7%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매
2회

실험 절차

5-Benzyloxy-2-[1-(4-chlorophenyl)-cyclopentylmethyl]-6-hydroxypyrimidine-4-carboxylic acid cyclopropyl-(2-hydroxyethyl)-amide (326) (90 mg, 0.17 mmol) and triphenylphosphine (90.5 mg, 0.35 mmol) were taken up in dichloromethane (3 ml) at room temperature followed by the slow addition of diisopropyl azodicarboxylate (52.34 mg, 0.26 mmol) and stirring for 1 h. Dichloromethane (15 ml) was added to the reaction mixture, which was subsequently washed with water (10 ml) and brine (10 ml). The organic part was dried and concentrated under reduced pressure. The obtained residue was purified by normal silica column using 30% ethyl acetate in hexane to get 9-benzyloxy-6-[1-(4-chlorophenyl)-cyclopentylmethyl]-2-cyclopropyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (327) (130 mg, 56%; 2 steps) as a sticky yellow solid.

후처리

  1. washwas subsequently washed with water (10 ml) and brine (10 ml)
  2. customThe organic part was dried
  3. concentrationconcentrated under reduced pressure
  4. customThe obtained residue was purified by normal silica column

출처 및 근거

ORD 기록
ord-92f87f250dad4fa2a5878afc5ac2d83c
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09045486B2

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