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Sodium Cyanide → 1-(3-Iodo-5-methoxy-4-propoxyphenyl)-4-(3,4,5-trimethoxyphenyl)-1,4-butanedione

HRID 1085632
ノート
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反応式

HRID 1085632 の反応式
[I:1][C:2]1[C:3]([O:12][CH2:13][CH2:14][CH3:15])=[C:4]([O:10][CH3:11])[CH:5]=[C:6]([CH:9]=1)[CH:7]=[O:8].[C-]#N.[Na+].CN(C)[CH2:21][CH2:22][C:23]([C:25]1[CH:30]=[C:29]([O:31][CH3:32])[C:28]([O:33][CH3:34])=[C:27]([O:35][CH3:36])[CH:26]=1)=[O:24]>CN(C=O)C>[I:1][C:2]1[C:3]([O:12][CH2:13][CH2:14][CH3:15])=[C:4]([O:10][CH3:11])[CH:5]=[C:6]([C:7](=[O:8])[CH2:21][CH2:22][C:23]([C:25]2[CH:26]=[C:27]([O:35][CH3:36])[C:28]([O:33][CH3:34])=[C:29]([O:31][CH3:32])[CH:30]=2)=[O:24])[CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8929Sodium CyanideHCID 4123063-(Dimethylamino)-1-(3,4,5-trimethoxyphenyl)propan-1-oneHCID 47701013-Iodo-5-methoxy-4-propoxybenzaldehyde

生成物 1

HCID 157180281-(3-Iodo-5-methoxy-4-propoxyphenyl)-4-(3,4,5-trimethoxyphenyl)-1,4-butanedione

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

実験手順

A solution of 5-iodo 3-methoxy-4-n-propoxybenzaldehyde (26 g, 0.08 mol) in DMF (75 ml) was added over 15 minutes to a stirred solution of sodium cyanide (4 g, 0.08 mol) in DMF (100 ml) at 35° C. After stirring for 20 minutes, a solution of 3-dimethylamino-1-(3,4,5-trimethoxyphenyl)-1-propanone (18 g, 0.07 mol) in DMF (100 ml) was added over 0.5 hour. The mixture was stirred at 35° C. for 1 hour and kept at room temperature overnight. It was poured into ice-cold 20% hydrochloric acid (2 1), and the solid was filtered, dried by suction, and taken up in ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, and the filtrate was evaporated to dryness. Crystallization from Et2O-hexane gave 1-(5-iodo-3-methoxy-4-n-propoxyphenyl)-4-(3,4,5-trimethoxyphenyl)-1,4-butanedione, m.p. 120°-121° C.

後処理

  1. stirringThe mixture was stirred at 35° C. for 1 hour
  2. waitkept at room temperature overnight
  3. filtrationthe solid was filtered
  4. customdried by suction
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. customthe filtrate was evaporated to dryness
  8. customCrystallization from Et2O-hexane

出典と根拠

ORDレコード
ord-27d1b38fc75848e2af2e078b3e9a6f68
出典データセット
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05010100

反応ノート

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