Acetic Anhydride → Acetic acid N-hydroxysuccinimide ester

HRID 1165118

反応式

HRID 1165118 の反応式
[OH:1][N:2]1[C:6](=[O:7])[CH2:5][CH2:4][C:3]1=[O:8].[C:9](OC(=O)C)(=[O:11])[CH3:10].C(N(CC)CC)C>O1CCCC1>[CH3:10][C:9]([O:1][N:2]1[C:6](=[O:7])[CH2:5][CH2:4][C:3]1=[O:8])=[O:11]

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 80170N-Hydroxysuccinimide

生成物 1

HCID 84460Acetic acid N-hydroxysuccinimide ester

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

N-Hydroxysuccinimide (17.33 g, 0.5 mol) was suspended in 120 ml tetrahydrofuran and cooled in an ice bath. Acetic anhydride (16 ml, 0.17 ml) and then triethylamine (22 ml, 0.16 mol) were added slowly. A solution formed, and then gradually a white precipitate appeared. After one half hour an equal volume of petroleum ether was added, and the crystalline product was collected. Yield 21.22 g (90%, mp 128°-130° C., lit. 15 mp 131°-132° C.). Analysis (C6H7NO4): calc. 45.87% C, 4.49% H, 8.91% N; found 45.86%, C, 4.31% H, 8.61% N.

後処理

  1. temperaturecooled in an ice bath
  2. customA solution formed
  3. customthe crystalline product was collected

出典と根拠

ORDレコード
ord-175619cc98d54932a3666a48487c1ff6
出典データセット
uspto-grants-1990_03
特許番号
US04908322

関連ノート

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