Water → HCID 21997580、化合物

HRID 1977261ノート

反応式

HRID 1977261 の反応式
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:19]=[CH:18][C:13]([C:14]([NH:16][NH2:17])=[O:15])=[CH:12][CH:11]=1.N1C=CC=CC=1.[CH3:26][O:27][C:28]([C:30]1[CH:38]=[CH:37][C:33]([C:34](Cl)=[O:35])=[CH:32][CH:31]=1)=[O:29].O>O1CCCC1>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:19]=[CH:18][C:13]([C:14]([NH:16][NH:17][C:34](=[O:35])[C:33]2[CH:32]=[CH:31][C:30]([C:28]([O:27][CH3:26])=[O:29])=[CH:38][CH:37]=2)=[O:15])=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 81850Methyl 4-(chlorocarbonyl)benzoateHCID 21997501HCID 21997501、化合物

生成物 1

HCID 21997580HCID 21997580、化合物収率 99.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 4-(6-methoxy-n-hexyloxy)benzohydrazide (106.82 g) and pyridine (162 ml) in tetrahydrofuran (1 L) at 0°‥5° C. was treated portionwise with 4-methoxycarbonylbenzoyl chloride 83.75 g) over 30 minutes. After a further 1 hour at 0°-5° C., and 2 hours at room temperature, tlc indicated completed reaction and the reaction mixture was poured into water (7 L). The resulting precipitate was collected by filtration, washed thoroughly with water, and dried under hi-vacuum at 50° C. to give N-[4-(6-methoxy-n-hexyloxy)benzoyl]-N′-(4-methoxycarbonylbenzoyl)hydrazine (171.0 g) as a white solid.

後処理

  1. custom2 hours
  2. customat room temperature
  3. customreaction
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed thoroughly with water
  6. customdried under hi-vacuum at 50° C.

出典と根拠

ORDレコード
ord-a42fcf94beca42839dc09aef7a3ec94b
出典データセット
uspto-grants-2001_05
特許番号
US06232290B1

反応ノート

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