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O-Xylene → 2H-1,5-Benzodiazepine-2-thione, 1,3-dihydro-4-phenyl-

HRID 1580551
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인쇄 미리보기

반응식

HRID 1580551 반응식
[C:1]1([NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH2:7].C1(C)C(C)=CC=CC=1.[C:17]([CH2:25][C:26](S)=[S:27])(=O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O1CCOCC1>O>[C:18]1([C:17]2[CH2:25][C:26](=[S:27])[NH:8][C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=3[N:7]=2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7237O-XyleneHCID 7243O-PhenylenediamineHCID 312751,4-DioxaneHCID 11138043HCID 11138043, 화합물

생성물 1

HCID 30329842H-1,5-Benzodiazepine-2-thione, 1,3-dihydro-4-phenyl-

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1.08 g of o-phenylendiamine, 10 ml of xylene and 1.96 g of benzoyldithioacetic acid (Thuillier et al - Bull. Soc. Chim. Fr. 1938 (1959) is refluxed for 1 hour under a stream of nitrogen. The reaction may also be carried out in water, alcohol or dioxane. After cooling, the precipitate is filtered, washed with ethyl ether, and crystallized from ethyl acetate. Yield 2 g, m.p. 228°-230°C.

후처리

  1. temperature1938 (1959) is refluxed for 1 hour under a stream of nitrogen
  2. customThe reaction
  3. temperatureAfter cooling
  4. filtrationthe precipitate is filtered
  5. washwashed with ethyl ether
  6. customcrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-578e21f2f5b84458b25b5a8d1fbdf87a
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03933793

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