Cyclopropylamine → HCID 43403632, 화합물

반응식

[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[CH2:7]OS(C1C=CC(C)=CC=1)(=O)=O.[CH:19]1([NH2:22])[CH2:21][CH2:20]1>>[CH:19]1([NH:22][CH2:7][CH:2]2[CH2:3][CH2:4][CH2:5][CH2:6][O:1]2)[CH2:21][CH2:20]1

참가 물질

반응물 2

HCID 69828Cyclopropylamine

HCID 12641003HCID 12641003, 화합물

생성물 1

HCID 43403632HCID 43403632, 화합물

반응 조건

온도: 110 °C

실험 절차

A mixture of toluene-4-sulfonic acid tetrahydro-pyran-2-ylmethyl ester (500 mg, 1.85 mmol) and cyclopropylamine (2 mL, 15 mmol) is heated overnight at 110° C. in a sealed tube. The crude mixture is concentrated and taken up in CH2Cl2. Water is added, the layers are separated and the aqueous one back extracted twice with CH2Cl2. The combined organic extracts are washed with brine, dried over Na2SO4, filtered and concentrated. TLC, Rf (CH2Cl2/MeOH 95:5)=0.3, MS (LC-MS): 156.2 [M+H]+.

후처리

concentrationThe crude mixture is concentrated
additionWater is added
customthe layers are separated
extractionthe aqueous one back extracted twice with CH2Cl2
washThe combined organic extracts are washed with brine
dry with materialdried over Na2SO4
filtrationfiltered
concentrationconcentrated

출처 및 근거

ORD 기록: ord-495aaec245784a8d89965adb21d256c8
출처 데이터셋: uspto-grants-2010_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07807709B2

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