HCID 86614260、化合物 → HCID 68829063、化合物

HRID 2099350ノート

反応式

HRID 2099350 の反応式
[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

参加物

4

反応物 1

HCID 86614260HCID 86614260、化合物

生成物 1

HCID 68829063HCID 68829063、化合物収率 87.4%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒2 回HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f521f4a7c96f4fa39e9c7c9d8392b7e1
出典データセット
uspto-grants-2009_08
特許番号
US07569582B2

反応ノート

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