HCID 86614260, 화합물 → HCID 68829063, 화합물

HRID 2099350노트

반응식

HRID 2099350 반응식
[Cl:1][C:2]1[CH:41]=[CH:40][C:5]([CH2:6][C@@H:7]([NH:32]C(=O)OC(C)(C)C)[C:8]([N:10]2[CH:15]3[CH2:16][CH2:17][CH:11]2[CH2:12][CH:13]([N:18]([CH:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[C:19]([N:21]([CH2:24][CH3:25])[CH2:22][CH3:23])=[O:20])[CH2:14]3)=[O:9])=[CH:4][CH:3]=1>Cl.C(OCC)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][C@H:7]([C:8]([N:10]2[CH:15]3[CH2:16][CH2:17][CH:11]2[CH2:12][CH:13]([N:18]([CH:26]2[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]2)[C:19]([N:21]([CH2:22][CH3:23])[CH2:24][CH3:25])=[O:20])[CH2:14]3)=[O:9])[NH2:32])=[CH:40][CH:41]=1

참가 물질

4

반응물 1

HCID 86614260HCID 86614260, 화합물

생성물 1

HCID 68829063HCID 68829063, 화합물수율 87.4%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매2회HCID 3283Diethyl Ether용매2회

실험 절차

1.42 g of tert-butyl [(1R)-1-(4-chlorobenzyl)-2-(3-{cyclohexyl[(diethylamino)carbonyl]amino}-8-azabicyclo[3.2.1]oct-8-yl)-2-oxoethyl]carbamate are placed in 12 ml of 2N hydrochloric acid in diethyl ether. The reaction medium is stirred at ambient temperature for 3 h. 5 ml of 2N hydrochloric acid in diethyl ether are added and stirring is maintained for 16 h. After evaporation to dryness, the crude obtained is chromatographed on silica gel, elution being carried out with a 95/5/0.5 mixture of dichloromethane, methanol and aqueous ammonia. 1.03 g of N-[8-(4-chloro-D-phenylalanyl)-8-azabicyclo[3.2.1]oct-3-yl]-N-cyclohexyl-N′,N′-diethylurea are obtained.

후처리

  1. stirringstirring
  2. temperatureis maintained for 16 h
  3. customAfter evaporation to dryness
  4. customthe crude obtained
  5. customis chromatographed on silica gel, elution
  6. additionbeing carried out with a 95/5/0.5 mixture of dichloromethane, methanol and aqueous ammonia

출처 및 근거

ORD 기록
ord-f521f4a7c96f4fa39e9c7c9d8392b7e1
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07569582B2

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