Water → HCID 21997580, 화합물

HRID 1977261노트

반응식

HRID 1977261 반응식
[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

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 81850Methyl 4-(chlorocarbonyl)benzoateHCID 21997501HCID 21997501, 화합물

생성물 1

HCID 21997580HCID 21997580, 화합물수율 99.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-a42fcf94beca42839dc09aef7a3ec94b
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232290B1

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