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Ethyl 3-bromobenzoate → Ethyl 3-(2-(benzyloxymethyl)-2H-tetrazol-5-yl)benzoate

HRID 1820251
ノート
印刷プレビュー

反応式

HRID 1820251 の反応式
[CH2:1]([O:3][C:4](=[O:12])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7](Br)[CH:6]=1)[CH3:2].[CH2:13]([O:20][CH2:21][N:22]1[N:26]=[N:25][C:24]([Sn](CCCC)(CCCC)CCCC)=[N:23]1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C1(C)C=CC=CC=1.[Cu]I.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:13]([O:20][CH2:21][N:22]1[N:26]=[N:25][C:24]([C:7]2[CH:6]=[C:5]([CH:10]=[CH:9][CH:8]=2)[C:4]([O:3][CH2:1][CH3:2])=[O:12])=[N:23]1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 90488Ethyl 3-bromobenzoateHCID 113405612-((Phenylmethoxy)methyl)-5-(tributylstannyl)-2H-tetrazole

生成物 1

HCID 57888757Ethyl 3-(2-(benzyloxymethyl)-2H-tetrazol-5-yl)benzoate

試薬・触媒・溶媒 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 178418397
HCID 178418397、化合物
触媒
HCID 1140Toluene溶媒

実験手順

A solution of ethyl-3-bromobenzoate (0.47 g, 2.05 mmol) and 2-(benzyloxymethyl)-5-(tributylstannyl)-2H-tetrazole in toluene (20 mL) was degassed under vacuum and argon. To this solution was added copper (I) iodide (20 mg, 0.20 mmol) and tetrakis(triphenylphosphine)palladium(0) (115 mg, 0.10 mmol), and the mixture was again degassed under vacuum and argon. The flask and condenser were covered in foil to exclude light, and the reaction was heated at reflux temperature for 3 hours. After cooling to room temperature, the mixture was filtered and the filtrate was concentrated in-vacuo. The residue was purified over a 3.5×12 cm silica gel column, eluting with 5% then 10% then 15% ethyl acetate/hexanes to yield the title compound as a colorless oil which contained 5% of a tributyltin impurity. MS (ESI+)=339.22, (M+H)+. The oil was used as-is in the next step.

後処理

  1. customthe mixture was again degassed under vacuum and argon
  2. temperaturethe reaction was heated
  3. temperatureat reflux temperature for 3 hours
  4. filtrationthe mixture was filtered
  5. concentrationthe filtrate was concentrated in-vacuo
  6. customThe residue was purified over a 3.5×12 cm silica gel column
  7. washeluting with 5%

出典と根拠

ORDレコード
ord-6feeb0927652433d93bdbd7b94b6b7e1
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07601844B2

反応ノート

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