Sulfuryl chloride → 6-Chloro-2-benzothiazolamine

HRID 1284597ノート

反応式

HRID 1284597 の反応式
[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

参加物

4

反応物 2

HCID 24648Sulfuryl chlorideHCID 7358434-Chlorophenyl-2-thiourea

生成物 1

HCID 72266-Chloro-2-benzothiazolamine収率 85%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-f5846bc2010e4544b29535946ac5f83e
出典データセット
uspto-grants-1986_01
特許番号
US04563533

反応ノート

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