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Methyl iodide → 6-(2-benzyloxy-6-chloro-pyridine-4-carbonyl)-3,4-dimethyl-3H-benzoxazol-2-one

HRID 469320
ノート
印刷プレビュー

反応式

HRID 469320 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[C:13]([C:15]([C:17]2[CH:26]=[C:25]([CH3:27])[C:20]3[NH:21][C:22](=[O:24])[O:23][C:19]=3[CH:18]=2)=[O:16])[CH:12]=[C:11]([Cl:28])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.I[CH3:30]>CN(C=O)C>[CH2:1]([O:8][C:9]1[CH:14]=[C:13]([C:15]([C:17]2[CH:26]=[C:25]([CH3:27])[C:20]3[N:21]([CH3:30])[C:22](=[O:24])[O:23][C:19]=3[CH:18]=2)=[O:16])[CH:12]=[C:11]([Cl:28])[N:10]=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

4

反応物 2

HCID 6328Methyl iodideHCID 581811156-(2-benzyloxy-6-chloro-pyridine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one

生成物 1

HCID 581811066-(2-benzyloxy-6-chloro-pyridine-4-carbonyl)-3,4-dimethyl-3H-benzoxazol-2-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Under a nitrogen atmosphere and while cooling with ice 220 mg (5.06 mmol) sodium hydride (55%, suspension in mineral oil) were added to 2.00 g (5.07 mmol) 6-(2-benzyloxy-6-chloro-pyridine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one in 10 mL DMF. The reaction mixture was stirred for 30 min at RT. Then 0.312 mL (5.06 mmol) iodomethane were added and the mixture was stirred overnight at RT. The reaction mixture was poured onto water and the precipitated product was suction filtered, washed with water and dried. The residue was stirred with diethyl ether, suction filtered and dried.

後処理

  1. stirringthe mixture was stirred overnight at RT
  2. additionThe reaction mixture was poured onto water
  3. filtrationfiltered
  4. washwashed with water
  5. customdried
  6. stirringThe residue was stirred with diethyl ether, suction
  7. filtrationfiltered
  8. customdried

出典と根拠

ORDレコード
ord-f2c114a7a7fe4764b59b69caa2526c50
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629137B2

反応ノート

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