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

HRID 589360ノート

反応式

HRID 589360 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][C:14]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[N: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.CO.O.[OH-].[Li+].Cl>O1CCCC1.O>[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][C:14]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[N: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

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 89590282ethyl 2-[3-[4-(4-chlorobenzamido)benzyl]-1H-indazol-1-yl]acetate

生成物 1

HCID 715718292-[3-[4-(4-chlorobenzamido)benzyl]-1H-indazol-1-yl]acetic acid収率 74.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl 2-[3-[4-(4-chlorobenzamido)benzyl]-1H-indazol-1-yl]acetate (100 mg, 0.223 mmol) was dissolved in 3 mL tetrahydrofuran, and 1 mL methanol, 3 mL water were added. In an ice bath was, 47 mg (1.12 mmol) lithium hydroxide monohydrate was added. I was moved to be at room temperature and reacted for 10 minutes. The reaction was monitored to be complete by TLC. Diluted hydrochloric acid was added to adjust pH to be acidic. Water was added, pumping filtered, dried to obtain a white solid 70 mg, at a yield of 74.9%

後処理

  1. customIn an ice bath was
  2. customto be at room temperature
  3. customreacted for 10 minutes
  4. filtrationpumping filtered
  5. customdried

出典と根拠

ORDレコード
ord-c24f70785ba045d1acc62f7efbece5b4
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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