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

HRID 2234500ノート

反応式

HRID 2234500 の反応式
[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

参加物

4

反応物 1

HCID 21882609tert-butyl N-(4-pyrrolidin-1-ylcyclohexyl)carbamate2 回

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 6422Trifluoroacetic acid溶媒

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-e58a8e05d0fa4b629029aa8b580a8f41
出典データセット
uspto-grants-2010_05
特許番号
US07709471B2

反応ノート

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