Hydrochloric Acid → 4-[6-(Cyclopentyloxycarbonyl)amino-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl]-3-methoxybenzoic acid

HRID 1723212노트

반응식

HRID 1723212 반응식
O.[OH-].[Li+].[CH:4]1([O:9][C:10]([NH:12][C:13]2[CH:14]=[CH:15][C:16]3[O:21][CH2:20][CH2:19][N:18]([CH2:22][C:23]4[CH:32]=[CH:31][C:26]([C:27]([O:29]C)=[O:28])=[CH:25][C:24]=4[O:33][CH3:34])[C:17]=3[CH:35]=2)=[O:11])[CH2:8][CH2:7][CH2:6][CH2:5]1.Cl>CO.O>[CH:4]1([O:9][C:10]([NH:12][C:13]2[CH:14]=[CH:15][C:16]3[O:21][CH2:20][CH2:19][N:18]([CH2:22][C:23]4[CH:32]=[CH:31][C:26]([C:27]([OH:29])=[O:28])=[CH:25][C:24]=4[O:33][CH3:34])[C:17]=3[CH:35]=2)=[O:11])[CH2:5][CH2:6][CH2:7][CH2:8]1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 14763127Methyl 4-[6-(cyclopentyloxycarbonyl) amino-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl]-3-methoxybenzoate

생성물 1

HCID 147631294-[6-(Cyclopentyloxycarbonyl)amino-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl]-3-methoxybenzoic acid수율 67.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

Lithium hydroxide monohydrate (0.267 g.) was added as a solid to a stirred solution of methyl 4-[6-(cyclopentyloxycarbonyl)amino-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl]-3-methoxybenzoate (0.7 g.) in methanol (15 ml.) and water (2 ml.). The mixture was stirred for 12 hours then diluted with water and acidified to pH 3.35 with 3M hydrochloric acid. The precipitate which formed was isolated by filtration, washed with water and crystallized from methanol to give the title compound as a solid (0.457 g., 67%), m.p. 221°-222° C.

후처리

  1. customThe precipitate which formed
  2. customwas isolated by filtration
  3. washwashed with water
  4. customcrystallized from methanol

출처 및 근거

ORD 기록
ord-6357bbb8c4f040c7b75677845475aec0
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04859692

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