Hydrogen Sulfide → Thiobenzamide

HRID 466083

반응식

HRID 466083 반응식
CC([C:5]1[CH:6]=[C:7]([CH:10]=[C:11](C(C)(C)C)[C:12]=1OCOCCOC)[C:8]#[N:9])(C)C.C(N(CC)CC)C.N1C=CC=CC=1.[SH2:37]>>[C:7]1([C:8](=[S:37])[NH2:9])[CH:10]=[CH:11][CH:12]=[CH:5][CH:6]=1

참가 물질

5

반응물 4

HCID 402Hydrogen SulfideHCID 1049PyridineHCID 8471TriethylamineHCID 100416433,5-Bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzonitrile

생성물 1

HCID 683563Thiobenzamide

실험 절차

Into a solution containing 10.0 g (0.03 mole) of 3,5-bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzonitrile, 5.7 ml (0.04 mole) of triethylamine and 14.2 ml (0.18 mole) of pyridine, hydrogen sulfide gas is bubbled over 15 hours. The mixture is poured into ice water (110 ml), and an oily precipitate solidifies upon standing at 0° C. for 15 hours. The solid is thoroughly washed with water and filtered. Recrystallization from ethyl acetate and hexane gives 7.9 g (71%) of analytically pure 3,5-bis(1,1-dimethylethyl) -4-[2-methoxyethoxy)methoxy]benzenecarbothioamide, mp 113°-115° C.

후처리

  1. customis bubbled over 15 hours
  2. additionThe mixture is poured into ice water (110 ml)
  3. washThe solid is thoroughly washed with water
  4. filtrationfiltered
  5. customRecrystallization from ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-f75a7d5a54f648a180812aa487c0a582
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155122

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