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

HRID 589399ノート

反応式

HRID 589399 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%.

後処理

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

出典と根拠

ORDレコード
ord-9765130a361347f9ba1e22b136376228
出典データセット
uspto-grants-2016_01
特許番号
US09233098B2

反応ノート

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