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

HRID 34956노트

반응식

HRID 34956 반응식
[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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 704180878alpha-Benzyloxycarbonylaminoergoline

생성물 1

HCID 139664588alpha-Benzyloxycarbonylamino-6-n-propylergoline

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-89af1d7fd8184661a3b3f11df6dec6aa
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764517

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