一甲胺 → 他达拉非

HRID 540997

反应方程式

HRID 540997 反应方程式
C[O:2][C:3]([C@@H:5]1[CH2:17][C:16]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[NH:9][C:8]=2[C@H:7]([C:18]2[CH:26]=[CH:25][C:21]3[O:22][CH2:23][O:24][C:20]=3[CH:19]=2)[N:6]1[C:27](=[O:30])[CH2:28]Cl)=O.[CH3:31][NH2:32]>CO>[O:22]1[C:21]2[CH:25]=[CH:26][C:18]([C@@H:7]3[C:8]4[NH:9][C:10]5[CH:11]=[CH:12][CH:13]=[CH:14][C:15]=5[C:16]=4[CH2:17][C@@H:5]4[C:3](=[O:2])[N:32]([CH3:31])[CH2:28][C:27](=[O:30])[N:6]34)=[CH:19][C:20]=2[O:24][CH2:23]1

参与物

4

反应物 2

HCID 6329一甲胺HCID 68502869（1S，3S）-1-（1,3-苯并二恶唑-5-基）-2-（2-氯乙酰基）-2,3,4,9-四氢-1H-吡啶[3,4-b]吲哚- 3-羧酸甲酯

产物 1

HCID 110635他达拉非

试剂、催化剂与溶剂 1

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

实验过程

Cis-1-benzo[1,3]dioxol-5-yl-2-(2-chloro-acetyl)-2,3,4,9-tetrahydro-1H-beta-carboline-3-carboxylic acid methyl ester of Step 3 (30 g) was taken in methanol (450 ml). The resultant mixture was heated to 35° C. to 40° C. and aqueous methyl amine (27 ml; 40%) was added. The reaction mixture was stirred at 50° C. to 55° C. for 5 hours and then cooled to 10° C. to 15° C. with continuous stirring for 0.5 hours. The solid so obtained was filtered and dried to afford (6R,12 aR)-6-(1,3-benzodioxol-5-yl)-2,3,6,7,12,12a-hexahydro-2-methylpyrazino[1′,2′:1,6]pyrido[3,4-b]indole-1,4-dione.

后处理

  1. temperaturecooled to 10° C. to 15° C.
  2. stirringwith continuous stirring for 0.5 hours
  3. customThe solid so obtained
  4. filtrationwas filtered
  5. customdried

来源与证据

ORD记录
ord-a0cad8a8ee6240f0a111fc33167f056b
来源数据集
uspto-grants-2014_10
专利号
US08871932B2

关联笔记

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