Water → HCID 21997544, 화합물

HRID 1977262노트

반응식

HRID 1977262 반응식
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:31]=[CH:30][C:13]([C:14]([NH:16][NH:17][C:18](=O)[C:19]2[CH:24]=[CH:23][C:22]([C:25]([O:27][CH3:28])=[O:26])=[CH:21][CH:20]=2)=O)=[CH:12][CH:11]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:33].O>O1CCCC1>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:31]=[CH:30][C:13]([C:14]2[S:33][C:18]([C:19]3[CH:24]=[CH:23][C:22]([C:25]([O:27][CH3:28])=[O:26])=[CH:21][CH:20]=3)=[N:17][N:16]=2)=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 14817Phosphorus sulfide (P2S5)HCID 21997580HCID 21997580, 화합물

생성물 1

HCID 21997544HCID 21997544, 화합물수율 165.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of N-[4-(6-methoxy-n-hexyloxy)benzoyl]-N′-(4-methoxycarbonylbenzoyl)hydrazine (193.4 g) and phosphorus pentasulfide (113.34 g) in tetrahydrofuran (2.5 L) was heated to reflux for 1 hour then cooled to room temperature and poured into water (7 L). The resulting precipitate was collected by filtration, washed thoroughly with water then partially dried. The solid was added to 1:1 CH3CN—H2O (200 ml), sitrred then filtered. This procedure was repeated a further 2 times, and the resulting yellow powder washed thoroughly with acetonitrile (500 ml×5) then dried under hi-vacuum at 50° C. to give methyl 4-[5-[4-(6-methoxy-n-hexyloxy)phenyl]-1,3,4-thiadiazol-2-yl]benzoate (179.6 g) as a yellow powder.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 1 hour
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed thoroughly with water
  5. customthen partially dried
  6. additionThe solid was added to 1:1 CH3CN—H2O (200 ml)
  7. filtrationsitrred then filtered
  8. washthe resulting yellow powder washed thoroughly with acetonitrile (500 ml×5)
  9. customthen dried under hi-vacuum at 50° C.

출처 및 근거

ORD 기록
ord-9599b8bfffbf4feeba657d23dc68960b
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232290B1

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