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Hydrochloric Acid → HCID 58490215、化合物

HRID 1395869
ノート
印刷プレビュー

反応式

HRID 1395869 の反応式
Cl.[OH:2][CH2:3][CH2:4][C:5](=[NH:9])OCC.C(O)(=O)C.[CH:14]([NH2:16])=[NH:15].O.NN.[N:20]([O-])=O.[Na+].Cl>O>[N:15]1[CH:14]=[N:16][N:9]=[C:5]([CH2:4][CH2:3][OH:2])[N:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 160693Formamidine acetateHCID 12653320HCID 12653320、化合物HCID 23668193Sodium Nitrite

生成物 1

HCID 58490215HCID 58490215、化合物収率 22.2%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

To a mixture of ethyl 3-hydroxypropanimidate hydrochloride (1 mmol, 153 mg) and formamidine acetate (5 mmol, 521 mg) was added hydrazine hydrate (1 mL) under an atmosphere of argon. After stirring at room temperature for 2 hours, the mixture was diluted with water (10 mL) and sodium nitrite (12.5 mmol, 0.86 g) was added. To this solution was added 2% aqueous HCl dropwise on an ice bath until the now pink solution reached a pH of 3. The aqueous solution was extracted with methylene chloride (5×25 mL), dried with magnesium sulfate, the solvent was removed by rotary evaporation, and then dried under vacuum to afford the product, 2-(1,2,4,5-tetrazin-3-yl)ethanol (28 mg, 22%), as a pink oil. LRMS-ESI [M+H]+ calcd. for C4H7N4O+: 127.06, found: 126.7.

後処理

  1. additionwas added
  2. extractionThe aqueous solution was extracted with methylene chloride (5×25 mL)
  3. dry with materialdried with magnesium sulfate
  4. customthe solvent was removed by rotary evaporation
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-329fffbaab16486a82f6b8e7f678260c
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08900549B2

反応ノート

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