Water → 2-{2-[1-(5-Chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethanamine

HRID 1039105

반응식

HRID 1039105 반응식
[N:1]([CH2:4][CH2:5][CH:6]1[CH2:8][CH:7]1[CH:9]1[CH2:14][CH2:13][N:12]([C:15]2[N:20]=[CH:19][C:18]([Cl:21])=[CH:17][N:16]=2)[CH2:11][CH2:10]1)=[N+]=[N-].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>C1COCC1>[Cl:21][C:18]1[CH:17]=[N:16][C:15]([N:12]2[CH2:13][CH2:14][CH:9]([CH:7]3[CH2:8][CH:6]3[CH2:5][CH2:4][NH2:1])[CH2:10][CH2:11]2)=[N:20][CH:19]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 11776TriphenylphosphineHCID 86666146HCID 86666146, 화합물

생성물 1

HCID 669270622-{2-[1-(5-Chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethanamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2-{4-[2-(2-azidoethyl)cyclopropyl]piperidin-1-yl}-5-chloropyrimidine from step 2 of this example (28 mg, 0,091 mmol) was dissolved in 0.821 mL THF. PPh3 (47.9 mg, 0.182 mmol) was added, followed by addition of 0.091 mL water. The reaction mixture was stirred at room temperature for 1 hour then 40° C. for 3 hours before cooled back to room temperature. The solvent was evaporated in vacuum. The residue was purified by column chromatography eluting with 10% 2M NH3-MeOH/ethyl acetate to give the titled compound. LRMS calc: 280.8; obs: 281.1 (M+1).

후처리

  1. temperature40° C. for 3 hours before cooled back to room temperature
  2. customThe solvent was evaporated in vacuum
  3. customThe residue was purified by column chromatography
  4. washeluting with 10% 2M NH3-MeOH/ethyl acetate

출처 및 근거

ORD 기록
ord-7da1855485bb4a1aa25a5360248006ab
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552022B2

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