Hydrochloric Acid → 3-Benzyloxy-8,9,10,11-tetrahydropyrazino[1',2':1,2]imidazo[4,5-c]quinolin-6-amine hydrochloride

HRID 1364071ノート

反応式

HRID 1364071 の反応式
[ClH:1].CO.[NH2:4][C:5]1[C:14]2[N:15]=[C:16]3[CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18][N:17]3[C:13]=2[C:12]2[C:7](=[CH:8][C:9]([O:29][CH2:30][C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)=[CH:10][CH:11]=2)[N:6]=1>O1CCOCC1>[ClH:1].[CH2:30]([O:29][C:9]1[CH:8]=[C:7]2[C:12]([C:13]3[N:17]4[CH2:18][CH2:19][NH:20][CH2:21][C:16]4=[N:15][C:14]=3[C:5]([NH2:4])=[N:6]2)=[CH:11][CH:10]=1)[C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 66958130tert-butyl 6-amino-3-benzyloxy-10,11-dihydropyrazino[1',2':1,2]imidazo[4,5-c]quinoline-9(8H)-carboxylate

生成物 1

HCID 669583983-Benzyloxy-8,9,10,11-tetrahydropyrazino[1',2':1,2]imidazo[4,5-c]quinolin-6-amine hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Hydrogen chloride (20 mL of a 4 N solution in 1,4-dioxane) and methanol (20 mL) were added to tert-butyl 6-amino-3-benzyloxy-10,11-dihydropyrazino[1′,2′:1,2]imidazo[4,5-c]quinoline-9(8H)-carboxylate (4.45 g, 9.98 mmol, prepared by the methods described in Example 368 Parts A through I), and the reaction was stirred at ambient temperature overnight. A precipitate was present and was isolated by filtration and washed with cold methanol. The solid was then recrystallized from methanol, isolated by filtration, washed with diethyl ether, and dried overnight under vacuum at 65° C. to provide 3.89 g of 3-benzyloxy-8,9,10,11-tetrahydropyrazino[1′,2′:1,2]imidazo[4,5-c]quinolin-6-amine hydrochloride as a white solid.

後処理

  1. customprepared by the methods
  2. customwas isolated by filtration
  3. washwashed with cold methanol
  4. customThe solid was then recrystallized from methanol
  5. customisolated by filtration
  6. washwashed with diethyl ether
  7. customdried overnight under vacuum at 65° C.

出典と根拠

ORDレコード
ord-46832aead838433ebc504dde06d4cfc6
出典データセット
uspto-grants-2011_02
特許番号
US07888349B2

反応ノート

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