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Hydrochloric Acid → HCID 57889538、化合物

HRID 1888110
ノート
印刷プレビュー

反応式

HRID 1888110 の反応式
[CH2:1]([O:8][CH2:9][N:10]1[N:14]=[N:13][C:12]([C:15]2[CH:16]=[C:17]([CH:23]=[CH:24][CH:25]=2)[C:18]([O:20]CC)=[O:19])=[N:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Li+].Cl>C1COCC1>[CH2:1]([O:8][CH2:9][N:10]1[N:14]=[N:13][C:12]([C:15]2[CH:16]=[C:17]([CH:23]=[CH:24][CH:25]=2)[C:18]([OH:20])=[O:19])=[N:11]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium Hydroxide2 回HCID 57888757Ethyl 3-(2-(benzyloxymethyl)-2H-tetrazol-5-yl)benzoate

生成物 1

HCID 57889538HCID 57889538、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of ethyl 3-(2-(benzyloxymethyl)-2H-tetrazol-5-yl)benzoate (653 mg, 1.93 mmol) in THF (10 mL) was treated with a 0.5 M aqueous lithium hydroxide solution (5.8 mL, 2.9 mmol), and the reaction mixture was stirred for about 16 h. Analysis by LC/MS indicated that the reaction had not gone to completion, so the mixture was treated with a 0.5 M aqueous lithium hydroxide solution (1 mL, 0.5 mmol), and the reaction mixture was stirred for an additional 6 hours. The THF was removed under reduced pressure, and the aqueous solution was treated with 1 N HCl (3.5 mL, 3.5 mmol). The resulting mixture was extracted 3× with ethyl acetate, and the combined organic phases were dried over sodium sulfate and concentrated in vacuo to yield the title compound as a colorless powder which was used as-is in the next step.

後処理

  1. stirringthe reaction mixture was stirred for an additional 6 hours
  2. customThe THF was removed under reduced pressure
  3. extractionThe resulting mixture was extracted 3× with ethyl acetate
  4. dry with materialthe combined organic phases were dried over sodium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f723ab8a813448d1b3e42d421d94c3e8
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501782B2

反応ノート

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