Hydrochloric Acid → HCID 21868368, 화합물

HRID 857546노트

반응식

HRID 857546 반응식
C([O:3][C:4](=[O:27])[CH2:5][N:6]1[CH:26]=[CH:25][C:10]([NH:11][C:12]([O:14][CH2:15][C:16]2[CH:24]=[CH:23][C:22]3[O:21][CH2:20][O:19][C:18]=3[CH:17]=2)=[O:13])=[N:9][C:7]1=[O:8])C.O.[OH-].[Li+].Cl>O1CCCC1.O>[CH2:15]([O:14][C:12]([NH:11][C:10]1[CH:25]=[CH:26][N:6]([CH2:5][C:4]([OH:27])=[O:3])[C:7](=[O:8])[N:9]=1)=[O:13])[C:16]1[CH:24]=[CH:23][C:22]2[O:21][CH2:20][O:19][C:18]=2[CH:17]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 68524231[4-N-(Piperonyloxycarbonyl)-cytosin-1-yl]-acetic acid ethyl ester

생성물 1

HCID 21868368HCID 21868368, 화합물수율 98.2%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of [4-N-(piperonyloxycarbonyl)-cytosin-1-yl]-acetic acid ethyl ester (6.40 g, 17 mmol) in tetrahydrofuran (30 mL) and water (60 mL) was added lithium hydroxide monohydrate (1.6 g) at room temperature. After stirring 20 min, the reaction mixture was acidified by adding 1 N HCl (40 mL). The precipitated solid was filtered off, washed with water (20 mL) and ethyl alcohol (20 mL), and dried in vacuo to give the desired product (5.8 g, 98%). 1H-NMR (500 MHz; DMSO-d6) δ 7.94 (d, 1H), 6.93 (d, 1H), 6.90 (s, 1H), 6.82 (s, 2H), 5.93 (s, 2H), 4.99 (s, 2H), 4.43 (s, 2H).

후처리

  1. filtrationThe precipitated solid was filtered off
  2. washwashed with water (20 mL) and ethyl alcohol (20 mL)
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-b296f965ed0147dc94ba501f931721b3
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07145006B2

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