Hydrogen Sulfide → HCID 14447407、化合物

HRID 1657703ノート

反応式

HRID 1657703 の反応式
[C:1]1([CH:7]([C:9]([O:11][CH:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])[NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(O[CH:28]=[S:29])C.S>O1CCCC1>[S:29]=[CH:28][NH:8][CH:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:9]([O:11][CH:12]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)=[O:10]

参加物

5

反応物 3

HCID 402Hydrogen SulfideHCID 11073343Methanethioic acid, O-ethyl esterHCID 131710294HCID 131710294、化合物

生成物 1

HCID 14447407HCID 14447407、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 15.9 g. (0.05 mol.) of α-phenylglycine, diphenylmethyl ester, and 9 g. of (0.1 mol.) of ethylthioformate in 50 ml. of tetrahydrofuran is stirred overnight at room temperature. Then a stream of hydrogen sulfide is passed into the solution for 10 minutes, the reaction mixture is permitted to stand overnight, then concentrated and petroleum ether is added to the residue. 16.9 g. of α-[(thioxomethyl)amino]benzeneacetic acid, diphenylmethyl ester, crystallizes. The crude product is recrystallized from methanol, m.p. 129°-130°.

後処理

  1. concentrationconcentrated
  2. additionpetroleum ether is added to the residue
  3. customof α-[(thioxomethyl)amino]benzeneacetic acid, diphenylmethyl ester, crystallizes
  4. customThe crude product is recrystallized from methanol, m.p. 129°-130°

出典と根拠

ORDレコード
ord-357c0323264d4f3faa38796271d59cae
出典データセット
uspto-grants-1976_06
特許番号
US03962229

反応ノート

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