Sulfuryl chloride → 6-Chloro-2-benzothiazolamine

HRID 1284597노트

반응식

HRID 1284597 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH2:11])=[S:10])=[CH:4][CH:3]=1.S(Cl)(Cl)(=O)=O>ClC1C=CC=CC=1>[NH2:11][C:9]1[S:10][C:4]2[CH:3]=[C:2]([Cl:1])[CH:7]=[CH:6][C:5]=2[N:8]=1

참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 7358434-Chlorophenyl-2-thiourea

생성물 1

HCID 72266-Chloro-2-benzothiazolamine수율 85%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

실험 절차

186.5 parts of 4-chlorophenylthiourea were suspended with stirring in 850 parts of chlorobenzene, and 185 parts of sulfuryl chloride were added uniformly with stirring at a temperature of 40°-45° C. within about 3 hours. After the immediately starting gas development had ceased, the suspension formed which could be stirred with difficulty only was liberated from the chlorobenzene by steam distillation. The remaining suspension of 2-amino-6-chlorobenzothiazolium chloride was adjusted to pH 8 with 25% ammonia solution, thus causing the crude 2-amino-6-chlorobenzothiazole to agglomerate to a tacky mass. By decantation and drying, 146.3 parts of 2-amino-6-chlorobenzothiazole containing about 85% of pure product were obtained (=124.4 parts of 100% product, 67.4% of th.).

후처리

  1. additionwere added uniformly
  2. customthe suspension formed which
  3. stirringcould be stirred with difficulty
  4. distillationonly was liberated from the chlorobenzene by steam distillation
  5. additionThe remaining suspension of 2-amino-6-chlorobenzothiazolium chloride
  6. customBy decantation and drying

출처 및 근거

ORD 기록
ord-f5846bc2010e4544b29535946ac5f83e
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04563533

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