Benzoyl chloride, 3-nitro- → HCID 86742197、化合物

HRID 1253247ノート

反応式

HRID 1253247 の反応式
[CH3:1][C@@H:2]([C@@H:10]1[C@@:14]2([CH3:31])[CH2:15][CH2:16][C@@:17]34[CH2:23][C@:22]53[CH2:24][CH2:25][C@H:26]([OH:30])[C:27]([CH3:29])([CH3:28])[C@@H:21]5[CH2:20][CH2:19][C@H:18]4[C@:13]2([CH3:32])[CH2:12][CH2:11]1)[CH2:3][CH2:4][C:5]([CH3:9])=[C:6]([CH3:8])[CH3:7].[N+:33]([C:36]1[CH:37]=[C:38]([CH:42]=[CH:43][CH:44]=1)[C:39](Cl)=[O:40])([O-:35])=[O:34]>N1C=CC=CC=1>[CH3:1][C@@H:2]([C@@H:10]1[C@@:14]2([CH3:31])[CH2:15][CH2:16][C@@:17]34[CH2:23][C@:22]53[CH2:24][CH2:25][C@H:26]([OH:30])[C:27]([CH3:29])([CH3:28])[C@@H:21]5[CH2:20][CH2:19][C@H:18]4[C@:13]2([CH3:32])[CH2:12][CH2:11]1)[CH2:3][CH2:4][C:5]([CH3:9])=[C:6]([CH3:7])[CH3:8].[N+:33]([C:36]1[CH:37]=[C:38]([CH:42]=[CH:43][CH:44]=1)[C:39]([O-:30])=[O:40])([O-:35])=[O:34]

参加物

4

反応物 2

HCID 8495Benzoyl chloride, 3-nitro-HCID 13920164Cyclobranol

生成物 1

HCID 86742197HCID 86742197、化合物収率 165.6%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
20 °C

実験手順

Cyclobranol (18 g, 0.04 mole) dissolved in pyridine (200 ml) was stirred and cooled in a bath of ice water, and to it was added m-nitrobenzoyl chloride (9.85 g, 0.053 mole). Then the mixture was warmed to 20° C. and continued to stir for 12 hours. After the reaction is complete the mixture was evaporated under reduced pressure. Ice cold water (200 ml) was added to the residue and crystals begans to appear. The crude crystals were separated by filtration and recrystallized from acetone-water (1:1, V/V), giving cyclobranol-m-nitrobenzoate (20.1 g), in a 83% yield. m.p. 206°-207° C.

後処理

  1. stirringto stir for 12 hours
  2. customwas evaporated under reduced pressure
  3. additionIce cold water (200 ml) was added to the residue and crystals
  4. customThe crude crystals were separated by filtration
  5. customrecrystallized from acetone-water (1:1, V/V)

出典と根拠

ORDレコード
ord-d562b69e6295487ca7c7b23d0697a100
出典データセット
uspto-grants-1988_05
特許番号
US04748161

反応ノート

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