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Triethylamine → N-Methyl-N'-(4,5,6,7-tetrahydro-1-benzothiophen-4-yl)urea

HRID 259313
ノート
印刷プレビュー

反応式

HRID 259313 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.C(N(CC)CC)C.[CH3:19][N:20]=[C:21]=[O:22]>C1C=CC=CC=1>[CH3:19][NH:20][C:21]([NH:11][CH:7]1[C:4]2[CH:5]=[CH:6][S:2][C:3]=2[CH2:10][CH2:9][CH2:8]1)=[O:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 12228Methyl IsocyanateHCID 173886004,5,6,7-Tetrahydrobenzo[b]thiophen-4-amine hydrochloride

生成物 1

HCID 20348942N-Methyl-N'-(4,5,6,7-tetrahydro-1-benzothiophen-4-yl)urea

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 1.89 grams (0.01 mole) of 4,5,6,7-tetrahydrobenzo[b]thiophen-4-amine hydrochloride in 20 ml. of dry benzene is stirred while 1.05 grams (0.01 mole) of triethylamine and 01.7 ml. (excess) of methyl isocyanate are added successively. Addition of the latter gives rise to an exotherm, and the mixture becomes very pasty. The mixture is kept at 45° C. for 1 hour, and after cooling to room temperature, the solid is collected, washed thoroughly with benzene and then with water. On drying, this gives 1.7 grams (81%) of product, melting point 183° C. to 186° C. Recrystallization from acetone gives 1.23 grams, melting point 187.5° C. to 189° C.

後処理

  1. additionAddition of the latter
  2. customgives rise to an exotherm
  3. customthe solid is collected
  4. washwashed thoroughly with benzene
  5. customOn drying
  6. customRecrystallization from acetone
  7. customgives 1.23 grams, melting point 187.5° C. to 189° C.

出典と根拠

ORDレコード
ord-ec8dc9a460f44e558e5199fcbe6e9bc3
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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