tert-butyl N-(4-pyrrolidin-1-ylcyclohexyl)carbamate → Cyclohexanamine, 4-(1-pyrrolidinyl)-, trans-(9CI)

HRID 2234500노트

반응식

HRID 2234500 반응식
[N:1]1([CH:6]2[CH2:11][CH2:10][CH:9]([NH:12]C(=O)OC(C)(C)C)[CH2:8][CH2:7]2)[CH2:5][CH2:4][CH2:3][CH2:2]1>C(Cl)Cl.C(O)(C(F)(F)F)=O>[N:1]1([CH:6]2[CH2:11][CH2:10][CH:9]([NH2:12])[CH2:8][CH2:7]2)[CH2:2][CH2:3][CH2:4][CH2:5]1

참가 물질

4

반응물 1

HCID 21882609tert-butyl N-(4-pyrrolidin-1-ylcyclohexyl)carbamate2회

생성물 1

HCID 21882596Cyclohexanamine, 4-(1-pyrrolidinyl)-, trans-(9CI)수율 74%

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 6422Trifluoroacetic acid용매

실험 절차

tert-butyl N-(4-pyrrolidin-1-ylcyclohexyl)carbamate (Intermediate 238; 222 mg, 0.83 mmol) was taken up in DCM (1.5 mL) and TFA (1 mL). The reaction mixture was stirred at ambient temperature for 3 hours, poured directly onto an SCX-3 cartridge (2 g), pre-wet with DCM. The cartridge was washed through with DCM (10 mL), followed by methanol (30 mL) and then eluted with 2M ammonia in Methanol (25 mL). Evaporation to dryness of the ammoniacal solution yielded the title compound as an amber coloured oil (103 mg, 74%)

후처리

  1. washThe cartridge was washed through with DCM (10 mL)
  2. washeluted with 2M ammonia in Methanol (25 mL)
  3. customEvaporation to dryness of the ammoniacal solution

출처 및 근거

ORD 기록
ord-e58a8e05d0fa4b629029aa8b580a8f41
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709471B2

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