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

HRID 1364071노트

반응식

HRID 1364071 반응식
[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

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-46832aead838433ebc504dde06d4cfc6
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07888349B2

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