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Potassium cyanate → N-(4,5,6,7-Tetrahydro-1-benzothiophen-4-yl)urea

HRID 259320
ノート
印刷プレビュー

反応式

HRID 259320 の反応式
Cl.[S:2]1[CH:6]=[CH:5][C:4]2[CH:7]([NH2:11])[CH2:8][CH2:9][CH2:10][C:3]1=2.[O-:12][C:13]#[N:14].[K+]>O>[S:2]1[CH:6]=[CH:5][C:4]2[CH:7]([NH:11][C:13]([NH2:14])=[O:12])[CH2:8][CH2:9][CH2:10][C:3]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11378442Potassium cyanateHCID 173886004,5,6,7-Tetrahydrobenzo[b]thiophen-4-amine hydrochloride

生成物 1

HCID 13036998N-(4,5,6,7-Tetrahydro-1-benzothiophen-4-yl)urea収率 22.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of 50 grams of 4,5,6,7-tetrahydrobenzo-[b]thiophen-4-amine hydrochloride (about 45 grams real, based on 90% purity) in 100 ml. of water is stirred at about 15° C., and a solution of 23.1 grams of potassium cyanate in 100 ml. of water is added dropwise. After completion of the addition, the mixture is warmed slowly to 70° C. to 75° C. and held for an hour. The mixture is cooled, and the white solid is collected by filtration and washed with water. The solid is air-dried, pulverized, and washed with acetonitrile. On drying, this gives 37.3 grams of crude product, which on treatment with about 1200 ml. of hot acetone gives 11.45 grams, melting point 200° C. to 204° C. of the title compound.

後処理

  1. additionAfter completion of the addition
  2. temperaturethe mixture is warmed slowly to 70° C. to 75° C.
  3. waitheld for an hour
  4. temperatureThe mixture is cooled
  5. filtrationthe white solid is collected by filtration
  6. washwashed with water
  7. customThe solid is air-dried
  8. washwashed with acetonitrile
  9. customOn drying

出典と根拠

ORDレコード
ord-eb11f542b42747ea8f466d8035fed330
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04036979

反応ノート

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