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Acetic Anhydride → HCID 71245377、化合物

HRID 1186017
ノート
印刷プレビュー

反応式

HRID 1186017 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH2:14][CH2:13][C:12]1([CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:16](=[O:26])[NH:17][C@@H:18]([C@H:23]([OH:25])[CH3:24])[C:19]([O:21][CH3:22])=[O:20])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CCN(CC)CC.[CH3:41][C:42](OC(C)=O)=[O:43]>C1COCC1.C(Cl)Cl>[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH2:14][CH2:13][C:12]1([C:16](=[O:26])[NH:17][C@@H:18]([C@H:23]([O:25][C:42](=[O:43])[CH3:41])[CH3:24])[C:19]([O:21][CH3:22])=[O:20])[CH2:27][C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=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 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 71245383HCID 71245383、化合物

生成物 1

HCID 71245377HCID 71245377、化合物収率 76.3%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Compound 4 (3 g, 6.60 mmol) was dissolved in THF (30 mL), Et3N (1.11 mL, 7.92 mmol) and Ac2O (742 mg, 7.26 mmol) were added at RT. The reaction mixture was stirred at RT for 2 h. The volatiles were evaporated under reduced pressure and the residue obtained was diluted with CH2Cl2 and washed with dilute HCl. The combined organic extracts were dried over Na2SO4 and concentrated under reduced pressure. The crude residue was purified by column chromatography using 30% EtOAc/Hexane as eluent to yield compound 5 (2.5 g, 76%).

後処理

  1. customThe volatiles were evaporated under reduced pressure
  2. customthe residue obtained
  3. washwashed with dilute HCl
  4. dry with materialThe combined organic extracts were dried over Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customThe crude residue was purified by column chromatography

出典と根拠

ORDレコード
ord-bf5ebc82e0664112a529b0b23a89ccf5
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08673843B2

反応ノート

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