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

HRID 589370ノート

反応式

HRID 589370 の反応式
[Cl: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][CH:3]=1.O.[OH-].[Li+].O.Cl>O1CCCC1>[Cl:1][C:2]1[CH:3]=[CH:4][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]([OH:26])=[O:25])=[N:15]3)=[CH:11][CH:10]=2)=[O:7])=[CH:31][CH:32]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 89590262ethyl 2-[1-[4-(4-chlorobenzamido)benzyl]-1H-indazol-3-yl]acetate

生成物 1

HCID 715718312-[1-[4-(4-chlorobenzamido)benzyl]-1H-indazol-3-yl]acetic acid収率 96.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl 2-[1-[4-(4-chlorobenzamido)benzyl]-1H-indazol-3-yl]acetate (159 mg, 0.355 mmol) was dissolved in tetrahydrofuran (10 mL). In an ice bath, 10 mL aqueous solution dissolving lithium hydroxide monohydrate (42 mg, 1.0 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. It was filtered, and dried to obtain a white solid 144 mg, at a yield of 96.6%.

後処理

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

出典と根拠

ORDレコード
ord-297ae7fac4ff4159adb7787b56d196dd
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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