Hydrochloric Acid → 2-[1-[4-(6-methylnicotinamido)benzyl]-1H-indazol-3-yl]acetic acid

HRID 589399노트

반응식

HRID 589399 반응식
[CH3:1][C:2]1[CH:32]=[CH:31][C:5]([C:6]([NH:8][C:9]2[CH:30]=[CH:29][C:12]([CH2:13][N:14]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[C:16]([CH2:23][C:24]([O:26]CC)=[O:25])=[N:15]3)=[CH:11][CH:10]=2)=[O:7])=[CH:4][N:3]=1.O.[OH-].[Li+].O.Cl>O1CCCC1>[CH3:1][C:2]1[CH:32]=[CH:31][C:5]([C:6]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([CH2:13][N:14]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[C:16]([CH2:23][C:24]([OH:26])=[O:25])=[N:15]3)=[CH:29][CH:30]=2)=[O:7])=[CH:4][N:3]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 89590264ethyl 2-[1-[4-(6-methylnicotinamido)benzyl]-1H-indazol-3-yl]acetate

생성물 1

HCID 715719392-[1-[4-(6-methylnicotinamido)benzyl]-1H-indazol-3-yl]acetic acid수율 95.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl 2-[1-[4-(6-methylnicotinamido)benzyl]-1H-indazol-3-yl]acetate (258 mg, 0.60 mmol) was dissolved in tetrahydrofuran (20 mL), and in an ice bath, 10 mL aqueous solution dissolving lithium hydroxide monohydrate (76 mg, 1.81 mmol) was added. It was reacted at room temperature for 3 h, and the reaction was monitored to be complete by TLC. Water was added into the system, and adjusted to pH≈3-4 with diluted hydrochloric acid. A solid precipitated, which was filtered and dried to obtain a white solid 230 mg, at a yield of 95.4%.

후처리

  1. additionwas added
  2. customIt was reacted at room temperature for 3 h
  3. customA solid precipitated
  4. filtrationwhich was filtered
  5. customdried

출처 및 근거

ORD 기록
ord-9765130a361347f9ba1e22b136376228
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09233098B2

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