Benzoyl chloride, 3-nitro- → HCID 86742197, 화합물

HRID 1253247노트

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HRID 1253247 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 86742197HCID 86742197, 화합물수율 165.6%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
20 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d562b69e6295487ca7c7b23d0697a100
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04748161

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