Potassium Carbonate → 8alpha-Benzyloxycarbonylamino-6-n-propylergoline

HRID 34956ノート

反応式

HRID 34956 の反応式
[CH2:1]([O:8][C:9]([NH:11][C@H:12]1[CH2:26][C@H:25]2[C@@H:15]([CH2:16][C:17]3[C:27]4[C:20](=[CH:21][CH:22]=[CH:23][C:24]2=4)[NH:19][CH:18]=3)[NH:14][CH2:13]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:34](I)[CH2:35][CH3:36]>CN(C)C=O>[CH2:1]([O:8][C:9]([NH:11][C@H:12]1[CH2:26][C@H:25]2[C@@H:15]([CH2:16][C:17]3[C:27]4[C:20](=[CH:21][CH:22]=[CH:23][C:24]2=4)[NH:19][CH:18]=3)[N:14]([CH2:34][CH2:35][CH3:36])[CH2:13]1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 704180878alpha-Benzyloxycarbonylaminoergoline

生成物 1

HCID 139664588alpha-Benzyloxycarbonylamino-6-n-propylergoline

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A suspension of 17.5 g (ca. 46 mM) of 8α-benzyloxycarbonylaminoergoline obtained from step (c), 13.5 g potassium carbonate and 6 ml (62 mM) n-propyl iodide in 300 ml dimethylformamide is stirred for 18 hours at room temperature. The mixture is filtered and concentrated in a rotary evaporator. The residue is treated with methylene chloride and shaken with water. The organic phase is dried over sodium sulphate, filtered and concentrated to give the crude heading compound.

後処理

  1. filtrationThe mixture is filtered
  2. concentrationconcentrated in a rotary evaporator
  3. additionThe residue is treated with methylene chloride
  4. stirringshaken with water
  5. dry with materialThe organic phase is dried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give the crude

出典と根拠

ORDレコード
ord-89af1d7fd8184661a3b3f11df6dec6aa
出典データセット
uspto-grants-1988_08
特許番号
US04764517

反応ノート

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